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How To Manufacture The D Enantiomer Of How To Manufacture The D Enantiomer Of Phenylaminopropane, And 3, 4, methyl-ene-dioxymeth-phenylaminopropane Re: DETAILED METHODS for NON-CHEMISTS METHamphetamine PRECURSS CLEANING/wk UP Extractomania... by Ozbee friends. edited by Placebo INDEX Equipment 2: Ingredients 3: Method step 1: step 2: step 3: step 4: step 5: step 6: 4: Acid/Base 5: HCl-Gassing 6: Note Equipment Various jars, glass vessels, beakers etc PH paper, electronic PH tester Filter paper coffee filters A strainer that will fit your filters nicely, so that you get better surface area then a funnel Hair dryer, heat lamps Hot plate, no open flames, only heat elements Separate funnel, similar, tube to siphoIngredients -Pills containing psuedo-ephedrine HCl ephedrine HCl. -NaOH/Sodium Hydroxide / caustic soda / strong base / lye . -Epsom salts that have been baked in oven 200 c f an hour to dry. -Methanol -Acetone -Toluene -Distillated wate Method e : If pills have red coating, put in jar, with acetone, shake until red coating is dissolved then continue as below. Step 1: First, put your pills in a jar. Add methanol about double the volume of the pills. Cap the jar shake till they break apart.
Leave to sit f a few hours shaking every 1 / 2 hour. Let settle into 2 nice layers then siphon decant off top layer. No need to get it all as we will do this 2 me times to be sure get all that pseudo. step 2: Once you have done it 3 times have the 3 lots of methanol from above, put them together put in freezer.
You want to get it real cold, near freezing then filter it thru a very fine filter, this may take some time if you dont have a vacuum filtration setup but thats ok, we aint in a hurry. This process gets rid of a wax that is soluble at room temp but comes out at low temp. step 3: e : This step is necessary only speeds things up. After the chilled filter, we will reduce the volume of methanol / pseudo solution. So, with good ventilation a fan blowing over pot, just reduce the volume of methanol, but till you see crystals anything. Just reduce it to a manageable amount, we just want a saturated solution, youll ice it thicken a bit.
Stop, take it off. step 4: Now you want to pour a thin film of this methanol / psuedo solution out on a more glass table f fast evaluation, you could just leave it laying around a couple of days let nature take its course, it does make pretty crystals. Scrape all your crystals up when they are dry put into are clean pyrex vessel. step 5: Now pour Toluene, about double your psuedo volume dry / anhydrous use your epsom's! over your powdered psuedo, heat till just be boiling with your fan blowing over it. Boil f 5 mins then filter.
Repeat this with fresh toluene until when you boil toluene it stays clear. To be sure of toluene doing its job, after filtering, add water to toluene be discarding youll see the censored come out. step 6: Next you can do an acetone wash, by putting your psuedo some acetone in a jar, shake filter. Dry pseudo you should have censored in clean pseudo HCl This procedure, rids the pills of: MCC waxes polymers lactose most censored !
BUT, povidone! Me on that later. You may choose to react your psuedo now. Or do an A/B acid / base extraction, basicly turn it into a freebase, oil. keep in mind... If you do an A/B now, you may lose some psuedo to the povidone.
So what are the choices? well, povidone is known to go thru Hi/RP, no problem, but must be steam distilled out after. which is a good thing coz you got no seperation's emulsions the cleanest meth around. Povidone is bad because povidone is known to as hold amines. It depends on what reaction your doing A/B: Ok, get your nice dry white powder add about equal part water. Now make up a 20 % NaOH solution 4 parts DH 2 O: 1 part NaOH.
Add Toluene to water / pseudo solution about equal to water volume. Yes, toluene first, it gives the pseudo somewhere to go instead of being burned by the base which can break it up turn it into aziradines! toxic! Add NaOH solution to water / pseudo /toluene solution till PH 13, remember to test PH of water toluene! Now shake the jar up very well let settle into layers.
Seperate toluene layer. Repeat this process 3 times combine all your toluene. You can wash the toluene / pseudo freebase with water now, if you like, seperate again. Now you can either, evaluate toluene f freebase crystals, you need to turn the freebase into a Hcl salt again. So you can add fresh DH 2 O about 2 mL f each gram of pseudo to your toluene drop HCl acid slowly with shaking each time into the toluene.
Check pH all the time stop just be neutral. Shake again, recheck, this is very tricky takes patience. Now seperate the water from the toluene. Now you can evaluate your water to get your pure pseudo HCl. You can repeat this are 1 2 times get a little me Gassing, Gassing makes things easier coz you just gas it, filter there your crystals, but it is tricky to get the hang of it Hydrogen Choice is dangerous! It will burn your censored in lungs instantly if inhaled too much of it!
You need to pipe HCl gas into your jar full of toluene pseudo freebase, but the gas your toluene must be dry: no water, everytime the gas fms crystals it will be reabsorbed by the miniscule amounts of water. If you dont know how to extract, you shouldnt play with gas yet. If you know how to gas then read on So, you need to dry your toluene / per solution with pre-baked epsom salts to as the water, then filter them out. Then gas your solution you will see a snow stm be your very eyes. Then just filter dry crystals. But still may contain povidone.
Post merely f informational purposes. I havent done anything illegal n should you. METHamphetamine synthesis I. -Placebos compilation of the Cure by Ozbee clean-up of sudafed other ephedrine pills various RP/I 2 red phosphorus / elemental iodine, pure, crystals methods. placebo Hive Researcher 07 - 04 - 00 11: 04 Go to what! Ok, this is a compilation of many peoples methods. I believe this to be the best, simplest, fastest, cleanest method f producing meth-amphetamine, in the highest yields possible f RP/I 2 /E reaction.
Remember, each every step gives small losses, this method has the least steps! It is a culmination of effects by work, CHEMMAN, maybe a few tiny touches by me. I re-iterate, I dont want any congratulations except f the write-up itself. You will need these things, no substitutions allowed. If you cant get this censored , you aint ready to make the best Go-Go in town. This is a refinement of all methods, the next step up from Push Pull, but nobody should be discouraged from attempting this, as you will probably find it easier.
pH paper isnt even necessary. This post is one method from Go to what. This post has to be followed from Go to what. Otherwise you can run into trouble, as povidone is removed in this extraction. It will be removed at the end.
Each step was chosen to complement the next. Under? Read on... Index: 1: Equipment 2: Reagents 3: Extraction of per 4: Reaction 5: Steam distillation 6: Crystallisation Equipment: Various jars 2 L pyrex vessel 2 L 2 neck round flat bottom flask 1 condenser, I recommend a coil condenser but a Liebig will suffice. 1 sloping splash head better, a steam distillation sloping splash head.
A steam pressure cooker, that has a release-valve on top. Hotplate, electric of course. Filter paper, Buchner vacuum would be nice too. Thermometer. 1 Glass stopper. Lengths of clear pvc tubing.
Pot with vegetable oil, which can fit your reaction vessel. Reagents: Iodine crystals. Red Phosphorus. Pseudo-ephedrine, ephedrine. Methanol.
Toluene. Acetone. NaOH. All must be clean anhydrous. Ice. Extraction of per: This method will deal with the HCl salt of per, a streamlined version of the Cure.
All pills are dumped into a large jar double of this pills-volume in the fm of methanol poured on top. This is stirred vigorously let st to settle thereafter, in the fridge seems to speed it up. After the top methanol layer has cleared it is carefully decanted off. This procedure is repeated 3 times. All methanol pulls are put together the methanol boiled off on a hotplate. As methanol gets down to the last little bit, it is taken off the heat.
Then a prior of acetone, twice your remaining liquid is dropped in. This fce's the per crystals to crash out. Then the remaining liquid is carefully evaded off. washes: Now you have your crude / dirty per HCl.
Next we will be doing successive toluene washes. Put your per crystals in a pyrex heat proof glass. Now add toluene to a safe level that can be lightly boiled on the hotplate. After about 5 mins boiling with stirring, take off the heat let it settle a minute. Now carefully pour off toluene into a filter to catch any remnants of per that may follow. Now if you get the toluene that has our contaminants in it add some water, you will see the crap, crash from the toluene into the water.
This is the crap that came thru with the methanol pull. So as we continue to do multiple toluene washes, we will continue to test the toluene after pouring it off, to see how we are progressing with the cleanup. when we have reached a point where no crap comes out of the toluene, with the addition of water, then we are ready to try acetone. Usually about 3 boils in toluene, but of course it depends how much your using. So, as be we will add a prior of acetone boil lightly. Now when we pour off the acetone, we will add a tiny amount of water some NaOH.
This is our final test, when you do this no crap falls out of acetone you are ready. This will be the cleanest per you have ever seen, guarenteed! , yields should be 90 % if your carefull! 95 % is good. Reaction: Smallest reaction to be attempted, especially by newbies, is 1 oz of per, so that even taking into account sloppiness, lack of experience losses along the way, you should get some product. Ratios of reagents are.
E: I: RP aka, equal amounts of Iodine per, a one third amount of RP. This is calculated on a weight basis, can be scaled up down as necessary, e. g. 60 gmE/ 60 gmI 2 / 20 gm RP 120 gmE/ 120 gmI 2 / 40 gm RP etc etc. First prepare yourself an isobath. Yes, ice cubes water in a sink bucket.
Now, many will say you should add this first that first. well, after much reading of different peoples methods, I say. Chuck the whole shebang in together, while your flask is on ice, lift swirl ingredients together, while maintain on ice. Put your condenser on top start water running thru, from bottom to top.
Now, the idea is to get the reaction going in the most controlled way possible, you want to let the reagents react in the container vessel fixed in the isobath, if at all. Then move vessel from isobath to room temp. If things look like theyre going too fast, put back in ice bath, you want to keep the reaction going but only at a nice slow, controlled pace. This is also necessary to control vapour in the condenser! Thick dis-could smoke is bad, plumes of smoke will escape from condenser. Let things progress at a nice slow pace, as things slow too much, you can start applying heat.
So prepare an oil bath bring to about 50 C, if there is no me action in your vessel. You can move it to the oil bath, the same goes f it as be, when things slow down. Adjust heat up, to say 100 C then 150 C f one hour, to make sure reaction has completed. The whole time you should be watching to keep a nice reflux going, too much vapour is escaping from condenser. Now remove from heat disconnect condenser, add ice water to quench reaction. The reason f ice water is to calm the reaction down when NaOH is added.
Its up to you if you want to filter out RP leave it in untill the end. I would leave it, it will be washed nicely by next process be easier to filter. Now add lots of NaOH to bring reaction mix to + 14 pH. You can over-basic, as meth wont be destroyed, its a tough MF! Steam Distillation: Now you need to set up your glassware f steam distillation.
Attach the steam distillation sloping splash head to top hole of flask, attach plastic hose to steam inlet the other end on the release valve of the pressure cooker that is full of water. Attach condenser on the end of splash head, rig the whole up so it stays up. Place a jar at the end of condenser to catch our distillate. You want to heat both the pressure cooker, the reaction flask. Sit back get ready f one of the most beautiful sights smells. The meth freebase that is sitting on the top of your aqueous layer in the flask will vapours be carried across be condensed in the condenser trickle down into your jar.
It will sit atop of a bottom layer of water. After the last of the oil has come across, change jars leave the setup to run f are hour, just to make sure you got it all. Any povidone from the pills will be stick behind in the reaction vessel. It has been ed that some polymer that may have been left from extraction, may follow the steam. Crystallisation: Now we have a jar of water, with this sweet clear oil sitting on top. Next options are to add HCl acid slowly with stirring until the oil layer disappears, then evap the whole lot to get crystals.
Or, as I found, you may have some polymer that has come over with the steam, is now sitting in the water layer, it looks cloudy. I dont want to evap all that, it will just concentrate the censored in there, plus its very time consuming evading water, plus you risk losing some meth as the water evap's. I think you should just throw a little toluene into the jar, then seperate. Now your absolutly pure meth freebase is in your toluene! Now you can either gas, f instant the now clean meth, add minimal distillate H 2 O then acidify to pH 7, shake, seperate evap water f crystals. Repeat this step if you do it this way, as some me may come in a second go.
with this process from start to finish, you shouldnt need to re-crystalize, as your product should be the cleanest censored anybody has ever seen anyway. But you may want to, f the purpose of growing nice big crystals. In which case, add just enough hot methanol to dissolve all your meth then place in freezer. The secret is, the slower the evap, the bigger the crystals. So a nice slow room temp evap over several days might be fun. Enjoy, do attempt anything above, be you completely under what you are doing!
You must have a sound understand of the basics first! How to produce anhydrous = dry = water free! HCl gas using no special equipment f all your aviation steps of freebases by PsychokittyTo date I have never used Strikes Festers method f producing HCl gas. Reasons f this are as follows The necessity of laity glassware no OTC hardware. 2. what seems to be a messy procedure using table salt but I wouldnt know exactly as Ive never tried it. 3.
Difficult dismantling process at least it seems to be me difficult than mine. I dont remember the exact journal reference that inspired my method, but I do know that it is described somewhere in Inganic Syntheses Vol. I. Okay. First, here is what you need Beer bottle transparent. 2. Plastic baby syringe 15 ml capacity found at the pharmacy section at any grocery ste. 3.
Four so feet of ice-maker transparent-white polyethylene tubing found at the hardware ste. I dont remember the exact diameter size. All I know is that it IS the smallest size available. 4. One table-leg stopper rubber, beige black.
Are item of which I dont know the size. Just take your beer bottle into the hardware ste see which size fits snuggly on its top. 5. One aluminum tube that is the exact diameter size as the polyethylene tubing. Found at the hardware ste but dont know what they are used f. They are sometimes made of brass. 6. One bottle of sulfuric acid drain cleaner. 7.
One bottle of concentrated hardware ste muratec acid 32 %? Assembling the HCl general is easy Use the aluminum tubing to burrow two holes to the top of the table-leg stopper. Use a twisting motion while appling pressure f about a minute eventually the tube will pop through. 2. Place the table-top stopper over the top of the beer bottle. Itll fit snugly. 3. Insert the polyethylene tubing into the middle-most hole push through until the tubing hits the bottom of the beer bottle.
with swiss a knife cut off the polyethylene tubing about two inches from the top of the beer bottle. 4. Take the entire table-top stopper inserted with the polyethylene tubing off of the beer bottle. Pour into the beer bottle a volume of sulfuric acid about an inch high off of the bottom of the beer bottle. 5. Replace the table-top stopper / polyethylene tubing on top of the beer bottle. Insert the remaining tubing into the last hole of the stopper until about two inches into the bottle.
Cut tubing down to desired length. 6. Pour about twenty milliliters of concentrated HCl into a cup. Extract into baby syringe until syringe is full 15 mL. NO, the HCl will dissolve any part of the syringe in any way. NEITHER THE HCl N THE SULFURIC ACID wILL REACT wITH ANY PIECE OF HARDwARE USED IN THIS SYSTEM. THIS SET-UP HAS BEEN TESTED MANY TIMES wITH SUCCESS Insert the syringe into the middle tubing the one that extends to the bottom of the beer bottle.
End should be submerged in Sulfuric acid. If insertion is difficult, use a knife to scrape the inside of the tubing to allow the syringe to fit me easily. 8. Securing the set-up with a clamp of some st attached to a st is optional but desirable. 9. Have hy on the side a container full of water. The use of this set-up to gas ones solvent / amine is just as easy with right h, hold the tubing that will expel gas lower into the solvent / amine solution. 2. with left h slowly start to inject the HCl solution in the syringe into the sulfuric acid.
Once it hits the acid, there will be alot of fizzing foaming IMMEDIATELY HCl gas will be pumped into the solvent / amine solution. Foaming is sometimes a problem as it starts to reach the top of the beer bottle. Simple wait a while let it settle then continue. Sometimes certain brs of drain opener can cause excessive foaming. If this occurs, switch brs. 3. One syringe is usually enough f an amount of about 30 - 40 g of product, but if me is needed after all the HCl has been injected, slowly SLOwLY remove the syringe from the tubing, first be letting a crack of air into the system.
BEwARE that this is suddenly going to bring a min rush of HCl from the gassing tube so make sure that it is submerged when doing this step. To continue, refill the syringe proceed as described above. 4. Once the gassing is complete, leave the syringe ATTACHED to the injection tube submerge the gassing tube in the container full of water If the syringe is attached to the injecting tube, the following sequence will occur. weigh down the gassing tube somehow as it must remain submerged. In a few minutes about five the sulfuric acid will cool a bit causing a sucking-back of the water into the beer-bottle. This will happen very suddenly very fast, but to wry as the water will only go in as far as the top of the beer bottle.
This is actually an advantage as in this way one is able to dilute the remaining HCl gas the remaining sulfuric acid. Of course the bottle will get hot but if left aside f a few minutes it will eventually cool making opening the container dispensing with the acid solution an easy task. If the bottle is opened f whatever reason without the above acid dilution step, HCl gas will be everywhere. Hope this method will prove useful to you my fellow bees, it sure has been f me!
wISDOMwillwIRe: DETAILED METHODS for NON-CHEMISTS Methyl Man (Hive Researcher) 06 - 05 - 00 10: 40: METHYLMANs WRITEUPS of Me OH BENZO WACKER and MeNO 2 -Al-Hg. Consult these threads to avoid unnecessary questions: web /perl / show flat . pl? Cat = &# 038; Board = methods&# 038; N umber = 13991 &# 038; page = &# 038; view = &# 038; sb = &# 038; vc = 1 target = new web &# 038; view = &# 038; sb = &# 038; vc = 1 and /perl / show flat . pl? Cat = &# 038; Board = methods&# 038; N umber = 15667 &# 038; page = 0 &# 038; view = collapsed&# 038; sb = 5 target = new web 0 &# 038; view = collapsed&# 038; sb = 5 and /perl / show flat .
pl? Cat = &# 038; Board = methods&# 038; N umber = 31473 &# 038; page = 0 &# 038; view = collapsed&# 038; sb = 5 target = new web 0 &# 038; view = collapsed&# 038; sb Here they are, with minor changes from older versions for greater accuracy. Methyl Mans Me OH version of the benzo quinone wacker Materials: 400 mL Me OH (methanol) 50 mL distilled H 2 O 150 g p-Benzoquinone 2 g palladium (II) chloride (Pd Cl 2) 178 g saf role DCM (methylene chloride; dichloro methane) NaCl (non-iodized table salt) Sodium bicarbonate (baking soda) 5 % NaOH HCl (hydrochloric acid, from muratec acid) Magnesium sulfate drying agent (epsom salts baked in 400? XF oven for 2 hours) Method: 1. In a 2 L flask fitted with a reflux condenser and addition funnel place 400 ml Me OH, 50 ml dH 2 O, 150 g p-Benzoquinone and 2 g Pd Cl 2 and leave to stir for a minimum of 60 minutes. Note that a recent improvement has been discussed which involves stirring the Pd Cl 2 in the solvent (Me OH in this case) for several hours before adding the water and benzo quinone.
It is likely that this does enhance yields a bit by ensuring maximum efficiency of the Pd Cl 2? ? s catalytic action. Either way will work well, however. If you let the Pd Cl 2 stir alone for a while, when you then add the water and benzo quinone, let them stir for an hour as well before beginning the next step so as to ensure complete dissolution of the benzo quinone. 2.
Place 178 g saf role mixed with a bit of Me OH in an addition funnel. 3. Add saf role drop wise from the addition funnel over 60 minutes or more. However, when the addition is about 80 % finished, apply low heat just sufficient to start a mild reflux (cold water through the condenser). 4. After the saf role addition is complete, leave mixture stirring and refluxing for 8 hours. (If you must stop at this point and resume another day, be sure to put the mixture in the freezer, sealed well.
The raw ketone decomposes unless stored at freezer temperatures. ) 5. Filter out the solids present in the mixture, which are hydroquinone (the degradation product of the benzo quinone) and Pd Cl 2. This can be done by vacuum filtration or by simple gravity filtration with coffee filters. Many prefer gravity filtration with this synthesis because the solids produced in this reaction are very fine and are problematic to filter with vacuum. Don? ?
t try to recycle the Pd Cl 2, as it is too difficult to separate from the hydroquinone to be worthwhile. 6. Flood mixture with 1. 7 L 3 N (~ 10 %) HCl. (Heres the quick math: add 500 mL of 31 % HCl [muratec acid] to 1150 mL H 2 O to get 1. 65 L ~ 10 % HCl? Xclose enough for this purpose. ) 7. Extract flooded mixture with 3 portions of DCM (1 x 500 mL, 1 x 250 mL, 1 x 100 mL) in a large separately funnel.
The desired raw product, MDP- 2 -P (? ? ketone? ? ), migrates into the DCM as an oil. Separate the DCM/ketone layers and combine them. (Note: when you first hit it with the DCM you will probably observe a bit of scum which will float on top of the water layer, which will work its way down during these three extractions to appear as a blob of spongy semi-solid interface. It? ? s actually very mobile and easy to work around; simply avoid allowing it into your DCM separations.
The same thing will happen in your washes in steps 10, 11 and 12 below, but by then you will be quite the pro at working with it. ) 8. Extract water layer with a final small amount of DCM. 9. Add this final small DCM extraction to the combined oil/DCM solution from step 8. 10. Wash the ketone/DCM solution with saturated sodium bicarbonate in water twice (500 mL each wash). 11. Wash the ketone/DCM solution with saturated NaCl 3 times (400 - 500 mL each wash). (Note: as you do these bicarb and salt water washes, you should be seeing the ketone/DCM solution getting progressively more greenish colored; this is visible in the film of solution that runs down the inner surface of the sep funnel). 12. Wash the ketone/DCM solution 3 times with 500 mL 5 % NaOH (500 mL each wash).
If you did step 5, you will have a very easy separation. (Note: you should also see a very noticeable color change upon doing the first of these three washes wherein the ketone/DCM layer becomes a strange, thick reddish-brown, almost orange color. This happens as the NaOH pulls the majority of the solved hydroquinone into its layer, cleaning the ketone. The NaOH layer in the first wash will be very dark brown, almost black in fact. The next two will be a far lighter, watery, orangy color. ) 13.
Dry the ketone/DCM solution with ~ 50 g magnesium sulfate. 14. Distill off the DCM using mild heat on a water bath and ice-cold water through the condenser. This will take several hours. 15. Add 50 mL of high-oleic safflower oil (no additives! ! ) to the ketone oil as a buffer to prevent the ketone from scorching in the distilling flask. 16.
Vacuum distill the ketone / buffer oil mixture. This also will take a few hours, but not as long as distilling the DCM off did. 17. At 100 to 140? XC (wherever your particular vacuum dictates), a minor amount of saf role might come over. If your saf role-to-ketone conversion was good, there should only be a very small amount.
If it is only a few drops to a milliliter or two, you can leave it in, and not change / clean receiving flasks. If you are a stickler for purity, discard it. It will not harm anything later if you leave it in. But if it? ? s more than a couple of milliliters, get rid of it. 18.
At anywhere from 25 to 40? XC above the temperature your saf role usually comes over with the same vacuum, the ketone should begin coming over. You should get about 100 to 120 g ketone. The color of the ketone coming over will likely be a pale, fluorescent-looking greenish yellow.
In fact it looks not unlike anti-freeze? Xa similar? ? neon green. ? ? You can stop distilling when the rate of ketone coming over has slowed to an agonizing one drop per 90 seconds or so. At this point there is so little left that it is probably not worth your time to wait for a drop per 1. 5 minutes (it? ? s not worth mine anyway). 19.
Immediately store your precious fluid in the freezer in an airtight sealed flask or bottle. Happy cooking The MeNO 2 -Al-Hg reductive aviation according to Methyl Man Since the appearance of Ritter's writeup of this method in Total Synthesis II, much discussion has taken place about it but, it has sometimes seemed, little has been clarified. This is due in large measure to the sensitivity of this reaction to even the most minor changes in its many variables. With this writeup, I hope to provide a clearer view of the method and to allow others to benefit from the hard-won experience of someone (not me) whom well call Mr.
A. Ritter's original writeup, while inspiring, lacked details about the many nuances that, once understood, allow the amateur chemist to really understand this reactions dynamics. Thus I have tried with this writeup to help the neophyte who has only physical observations and scant written material to guide him (although I suspect and hope that it may even help a few more seasoned cooks as well). The first thing Id like you to look at is the array of interrelating variables in this reaction that make it so delicate. They are as follows the thickness / type of the aluminum 2) the consistency (i. e.
flat, ground, etc. ) 3) the amount of Hg Cl 2 used in relation to the amount of aluminum 4) the addition rate of the MeNO 2 /MDP- 2 -P 5) the size of the reaction vessel in relation to the scale of the reaction 6) the ability to effectively stir the reaction 7) the coldness of the water through the reflux condenser (yes, even that! ) The above factors are sort of submitted in an order of importance (# 1 being most important), but in reality they are all inextricably related. I observed firsthand the trials and tribulations of Mr. A as he struggled to match up the correct combination of ratios and conditions that would allow a smooth, consistent reaction and predictable results every time. Finally, after lots of frustration, confusion, losses, and the enda revelation, the perfect set of elements was hit upon and recorded.
The scale Mr. A chooses to perform this reaction on is half-scale to the scale in the Ritter writeup, which was 55 g aluminum and 50 g MDP- 2 -P. Therefore this writeup will illustrate the reaction on a scale of 27. 5 g aluminum and 25 g MDP- 2 -P. The subject found for his own personal reasons that this smaller scale was much easier to manage (not the least of which is that even with a huge 4 -liter separately funnel, at this smaller scale it gets pretty filled up! ).
Theres no doubt that the original larger scale can be successfully applied, although it would r require adjustments in the glassware capacity, stirring method, and probably other elements. MATERIALS and APPARATUS: 27. 5 g Reynolds Wrap Heavy Duty aluminum foil 25 g MDP- 2 -P 20 mL MeNO 2 of 99 +% purity 750 mL Me OH + 50 mL more for addition funnel + additional small amounts that will be needed later to thin the mixture 400 mg Hg Cl 2 2 -liter 2 -neck flat bottom flask reflux condenser (400 mm preferable) 250 mL or 500 mL addition or separately funnel cooling setup (bucket, water pump, tubing, 1 large bag ice) METHOD: 1. Weigh 27. 5 g of Reynolds Wrap Heavy Duty aluminum foil (NOTE: it HAS to be Reynolds and it MUST be the heavy duty stuff) and then tear it by hand or cut it with scissors into small rectangles approximately 1 by. 75. Settle down with this task with a good CD or TV show because it is tedious and may take about 1. 5 to 2 hours. 2.
With a coffee grinder, grind these pieces of foil for durations of about 10 seconds. Fill the coffee grinder only loosely (about two thirds full dont stuff it! That will adversely change the consistency of the ground foil). It will probably take about 4 to 5 loads in your grinder to do the whole amount of foil, depending on the size of your grinder. (In actuality, the foil does not get ground, but rather, each individual piece just gets compacted and compressed. If it is compressed too heavily, the inner surfaces of the foil nuggets may be rendered inaccessible to the Hg/Me OH solution, changing the timing of the amalgamation and maybe even causing an incomplete or failed reaction. ) When properly done, the foil should be in gnarled little nuggets about the size of long-grain rice grains and should look really tight and small. The smaller, the better for good stirring. 3.
Place a 3 sirdar in your 2 L flat bottom flask and onto your stir plate. Add the foil nuggets to the flask and then proceed to set up your glass, support and clamps so that the reflux condenser and addition / sep funnel are securely affixed and your flask is well-centered on the stir plate (this will be critical when you begin to attempt stirring! ). Also, prepare your cooling, i. e.
attach the inflow and outflow tubes to the reflux condenser. 4. Carefully add the 400 mg Hg Cl 2 to 750 mL Me OH to a tightly sealable bottle and shake to dissolve all Hg Cl 2. Set this solution aside. 5. Combine the 25 g MDP- 2 -P, 20 mL MeNO 2, and 50 mL Me OH and pour them into the addition / sep funnel. Rinse your beaker (or whatever you used) with a tiny bit of additional Me OH to get the residual ketone and add it to this MDP- 2 -P/MeNO 2 /Me OH solution. 6. Very slowly and carefully (w / gloves , glasses, long sleeves and a Hail Mary if youre Catholic), using a large funnel, pour the Hg Cl 2 /Me OH solution from step 4 down the condenser. 7.
Turn the stirring on full blast for a 5 -second burst to intimately mix the solution and the foil. If you have prepared the foil as described above, it will easily stir. Give it a few more 5 -second stirs over the next few minutes. I believe that doing this really helps facilitate the amalgamation process that is about to occur. 8. After about 5 minutes or so, you will begin to see bubbles popping up on the surface of the Me OH solution. At first they will be tiny, like champagne bubbles.
Then after a few minutes you will see them joined by larger bubbles closer to the size of those seen in boiling water. It is around this same time that the appearance of the aluminum will change from its normal shiny silver color and start to take on a dull gray look, accompanied by a gray cloudy look that begins forming in the Me OH. This is the magic moment when you want to begin dripping in your MDP- 2 -P/MeNO 2 /Me OH mixture. Set a drip rate of approximately 2 drops per second at this point and no faster. You can speed it up a bit later to accelerate the reaction if desired. 9. Place about 3 lbs ice into your bucket.
When you can feel exothermic warmth begin by feeling the outside of the flask, quickly add about 2. 5 liters water to the bucket (or an appropriate amount to make very ice-heavy ice water) and plug in the pump. 10. While monitoring the growing intensity of the bubbling amalgamation, turn on / off the stirring intermittently as you did earlier. This time it is to assure distribution of the added ketone / nitro methane in the reaction flask but also because the amalgamation seems to gain its vital momentum more effectively if given some significant blocks of time (meaning about 30 seconds at a time) in between stirring bursts. When the reaction is clearly starting to get vigorous and hot, crank the stirring to 10 and leave it on.
NOTE: This is where you can take advantage of Mr. As trial and error regarding this reactions parameters. If you used the kind of foil specified, prepared it as specified, used no more than the specified 400 mg Hg Cl 2, and used a 2 -liter and NOT a smaller flask, you can breathe easy knowing that the reaction is going to hum along nicely but will not get out of control, and will result in perfectly processed aluminum amalgam sludge. You may think that a 2 -liter flask is oversized for this reaction, but that is precisely the point.
The extra headroom in the glass provides a nice zone of breathing room for the reaction and facilitates good refluxing. Ive seen this reaction get out of hand in a 1000 mL flask, and it isnt pretty, believe me. Use the 2 -liter. 11. As the reaction progresses only a few minutes after the addition was started, you will observe that the aluminum is breaking up fairly rapidly.
This is good, as long as you have the ketone / nitro mixture dripping in at a good rate of about 2 drops per second. But be careful with the addition rate at this point, as a rate that is much faster than this could easily send the reaction into overdrive (not good). Your reflux should be unnervingly vigorous as the amalgamation really starts to pick up speed, with the Me OH dripping really fast down out of the condenser. I know its hard to believe, but this is what you want, this is good. Im telling you, LOTS of trial and error came before this writeup. Trust me.
You will also see sludge already starting to settle at the bottom and forming a ring on the glass around the top surface of the spinning mess. The consistency will get thicker by the minute. Add more ice to your bucket as needed. 12. At this point you can sort of control the reaction rate by slowing down or speeding up the addition rate a bit. Of course the reaction is already barreling along, so you wont want to speed it up much. The concept here is that you want the addition of the ketone / nitro methane to be paced neck-and-neck, as it were, with the breakdown of the foil as it amalgamates and gets turned into sludge.
In other words, you have to watch those two things and sort of adjust the addition so that they proceed at approximately the same rate. Its tricky, and imprecise, but with a little experience and intuition youll get the hang of it. Sure, you could be lazy and just leave the addition at a steady 2 drops per second the whole time, but if the amalgamation peters out way before your addition is finished, and you find yourself adding your beautiful ketone to impotent sludge, dont cry to me. The addition should take about 40 - 45 minutes in total, and as its finishing, the state of the aluminum should be about 95 % broken down. In fact the reaction should by now (~ 45 minutes after addition was started) look like a really thick, steely-gray chowder with only minor small slivers of undissolved aluminum visible if any at all.
You will probably even need to add an extra 20 - 30 mL of Me OH down the condenser at this point (or before) to help it keep stirring effectively. This is no problem. A note about color at this point is helpful too. Comparing successful reactions to failed ones, I have observed that there is a distinctive color to the mixture early on that indicates healthy amalgamation and foretells a successful run. At a point maybe 30 minutes or so post-addition, the reaction takes on a color that I would describe as being light steely gray with blue overtones. It is a hard thing to describe shades of gray, but I will try.
It is a light shade, akin to the color of common gray sweat pants, but like I say with a very slight suggestion of a blue hue in there as well. This is in contrast to what I saw in failures resulting from using too thick of aluminum and not enough Hg Cl 2, where a dark metallic gray with definite green overtones (from unrelated ketone) was noted. NOTE: Another point I would like to make about the timing of the addition against the breakdown of the aluminum is that Mr. A found that there was a definite spike curve to the amalgamation reaction which was easily observed by watching the reflux rate. That is to say, there is a peak that it builds up to and then comes down from.
At this scale, and using the exact materials described herein, that buildup to peak and subsequent slowdown occurs over approximately 25 minutes or sorry fast. So at only about 20 - 25 minutes after you first started feeling the amalgamation heating up, it will have slowed to a reflux of about 2 drops per second, after having been at a peak with a reflux rate so furious it is a stream, not drops. At one hour and 15 minutes after you first started the addition, the reflux will have slowed to a very calm 1 drop per 2 seconds or so. Finally, when A) the reflux has slowed to almost no reflux at all B) if you stop the stirring you do not see any small bubbles anymore C) no uneaten aluminum is visible and the solution is a thick, uniform gray soup, the reaction has essentially finished. It will reach this state at about one hour 45 minutes to two hours after addition was started. Nevertheless, you will leave it stirring happily for a total of three hours after the addition was finished to assure that the reaction has run its full course and the conversions that you desire have had ample time to take place.
In fact you should add a bit of external heat at the point where the addition has finished and the reflux slows down dramatically, because I? ? ve found that if one doesn? ? t, there might be a bit of aluminum that refuses to break down all the way which results in the later extraction being messier and much more of a hassle. One reason I bring this all up is that there has been lots of talk about how this reaction needs 8 hours or 24 hours or even 36 hours to run! But those time frames apply only in cases where much thicker aluminum is used, and / or in variations using methylamine and not nitro methane. Mr.
A was never successful in using thicker aluminum, and doesnt want to be! Why would someone want to make a reaction take any more time than it needs? Beats me! Im mystified! The approach illustrated in this writeup optimizes this reaction to finish in 3 hours 45 minutes from beginning to end, and it probably doesnt even need that much time. 13.
If you chose to apply external heat, turn it off at about 30 minutes before the targeted finish time. Otherwise you will have to wait an extra 30 minutes (at least) for it to cool for the next steps. 14. When finish time has arrived, dismantle your setup, set aside your reaction flask, and make 750 mL of a 35 % NaOH solution (750 mL H 2 O + 262. 5 g NaOH) and let it cool to room temp or below (safety glasses! ). 15. Into a separately funnel no smaller than 2000 mL capacity, pour your beautiful gray reaction mixture, being very careful to KEEP THE STIRBAR FROM FALLING IN to the sep funnel and breaking it (that would be ugly). If your mixture is really thick, you may need to add small amounts of Me OH to thin it to a pourable consistency.
This is perfectly fine. Wash the final residue out of the reaction flask with a few mLs of Me OH and add it to the funnel also. 16. Slowly pour the NaOH solution into the sep funnel (gloves and glasses! no excuses! ). Thats right, dont dump it in wholesale.
Basifying should be a gentle process. If you bully those molecules they may decide theyre being disrespected and choose not to cooperate. Adding the NaOH will cause the mixture to warm up a bit as the very last bits of the aluminum are dissolved, which is fine. Swirl it a couple times and give it about 10 minutes to cool down to something closer to ambient temperature. That yummy stinky methylamine smell tells you that the reaction was successful. 17. When the mixture in the sep funnel has cooled down, extract it once with 400 mL toluene followed by once with 100 mL toluene.
These are the critical moments for your yield now, so you be sure to shake long and hard (at least 3 minutes) during these extractions (I dont have to tell you to vent do I? ! ). The toluene / product layer will of course be on top since toluene floats on water. Also, be sure to give the separations ample time to happen (at least 15 minutes); it is easy to tell when its okay to separate because the interface of small toluene bubbles finally resolves and you have a nice clean line between the layers. If you like, do as Mr. A does and finish off with a final small extraction of 50 - 60 mL toluene just to get the last of the stuff.
NOTE: Your extractions will contain a tiny amount of the base / metal /garbage from the bottom layer; this is inevitable but easily worked around in this way: when you have collected your combined toluene / product extractions in a bottle, chill that bottle in the freezer for 30 minutes or so. When cold, the garbage gets a lot less mobile and it is easy to decant the toluene away from it. Just be vigilant while pouring the last 50 mL or so and avoid letting that glob of crap rejoin the toluene. Yeah, you will lose the very last 2 or 3 mL, but thats life. Alternatively, you could filter it through a paper towel, but you will still lose the same amount when the towel absorbs it. Just get over it and move on! 18.
If you havent already, drain the garbage layer out of your sep funnel into a storage bottle or something, and wash the garbage residue out your sep funnel with water. 19. Wash the toluene / product 4 times (or more) in your sep funnel with 400 or 500 mL H 2 O and a final time with 500 mL of a saturated NaCl solution to remove any traces of solved Hg Cl 2. 20. Dry your toluene / product solution with 30 g of your favorite drying agent (Mg SO 4 recommended) in an acetone-cleaned, heat-dried bottle for no less than 45 minutes (Mr. A is superstitious so he lets it sit for an hour).
Shake it a few times during this period. 21. Filter the solution and gas it with that good ol HCl bubbler setup. Be smart and use just enough muratec (31 % HCl) to wet the salt but not enough to make any puddles, and put a wad of drying agent wrapped in tissue paper in line somehow between the reaction flask and the tube leading to your pipette end. Weep with joy as a bumper crop of white precipitate crashes out of solution. Expected yield: approximately 20 - 21. 5 g raw odoriferous product that will purify via careful recrystallization to 17 - 18 g of beautiful snow-white MDMA! Aint life grand? ~~~Theres a methyl to my madness~~~ WISDOMwillWIRe: DETAILED METHODS for NON-CHEMISTS P 2 P METHAMPHETAMINE, racemic mix Materials: See MDMA, Isosafrole etc Chemicals: See MDMA, exept: Change MDP 2 P to P 2 P, Phenyl- 2 -propane.
Method: The original link is broken, or the file is deleted, so: Laptop. posted 06 - 23 - 99 01: 04 PM Member Making of d, l-Meth (Ice). Ingredients: ? 138 gram P 2 P = +/- 1 gram mole. ? 1000 ml Methanol (+ 10 % weight Methylamine gas dissolved in it = +/- 100 gram) = +/- 3 go. ? 36 gram Mg SO 4. 7 H 2 O, magnesium sulfate (dry at 300 C for 2 Hrs in oven to get Mg SO 4. 1 H 2 O) = to dry Methanol/M. A.
mix. ? 200 ml Silicagel balls +/- 3 to 5 mm (dry at 300 C for 2 Hrs in oven, changes to dark brown! ), = to attack 2 go H 2 O, during imine forming. ? 15 gram Na BH 4 as a reducing agent for the formed (water free! ) Imine. IMPORTANT: THE REACTION IS VERY SENSIBLE FOR ANY WATER (fluid or vapour in the air! ). First quickly crunch your pre-dried (oven, 300 C, 3 hrs. ) DRY Mg SO 4 to pop corn shaped rocks in a mortar, sieve the powder out, and directly put the rocks under max. mixing in the Methanol/Methylamine mix and close the pot to let no water from the air in.
Keep mixing for 10 minutes, then all the water will be taken up to the Mg SO 4. Let stand and wait till all the Mg SO 4 is on the bottom. Now quickly tap off the now DRY Me OH/MA mix in a 2 L reaction flask and close that one. Wash directly your empty pot with lots of water, to remove the smell of methylamine so you can safely store it.
Now add the 200 ml (measure in beaker, neglect the free spaces) DRY Silicagel beads (2 - 5 mm) and a magnetic mixer bar also in the 2 L flask and close again. Keep 2 L flask in Silicone-oil bath at 20 C. Silicone-oil only slowly warms up! Do not apply heat now, its only meant as a cooling medium in this stage. Now add SLOWLY via a dropping funnel the 138 gr P 2 P to the 2 L flask under strong mixing.
The temperature rises to 23 C during the (water free) Imine forming. The water from this reaction is taken up by the dried Silicagel! This takes 30 minutes. Let then mix for another 1 hour. The reaction mix color changes from light yellow to coffee+milk color. Temp = 23 C.
Stop mixing after this 1 hour and pour the fluid off into a 2 L glas erlenmeyer with flat bottom and add a mixer. The remaining Silicagel is washed 3 times with 50 ml DRIED (use silicagel) methanol, to catch the remaining Imine, and those 2 x 50 ml is also poured into the 2 L erlenmeyer. Now put the 2 L erlenmeyer on magn. mixer, in a ice cubes / methanol bath (- 10 C) and start strong mixing. Put a Funnel on top of 2 L erlenmeyer, in rubber ring. Now start adding, every 5 min. , a teaspoon full (flat off! ) of boro and wash in with minimum methanol.
After every spoonful, stopper the funnel loosely with a rubber stopper. This takes 2, 5 hrs. DO NOT exceed a temp of more then 20 C! ! You can add the next spoon at +/- 8 C. Solution color is light clear orange / brown . Let mix in total for 8, 5 hrs. (could perhaps be lot less hours, dont want to know: time is NOT money! ).
The total volume is +/- 1900 ml. Add then the mix to 5 L dest. water in a 10 L flask, under magn. mixing. The pH = 12. Add then 500 ml DiChloroMethane (DCM) and mix strongly for 30 min.
Let oil precipitate and a dark, honey-coloured layer of DCM+oil is on the bottom. Decant the waterpark with an aspirator + silicone tube. Fill the rest (water+DCM+oil) in a separator funnel and tap off only the DCM+oil = 550 ml. (DCM boiling point = 40 C). The leftover Mg SO 4 and boro salts stayed nicely in the waterpark. Then dry the DCM+oil with some DRY Mg SO 4 and decant in 2 L erlenmeyer. Wash this Mg SO 4 with some fresh, DRY DCM and add the DCM washings to the now dry DCM+oil.
Total volume DCM+oil = 1000 ml, colour is honey / red . Start now bubbling this 1000 ml with HCl-gas, while 2 L erlenmeyer stands in isobath on magn. mixer and mix strongly. Check pH frequently, proceed until pH 6. Pour the now acidified 1000 ml in a 2 L evap.
flask and put on Rotavap machine. Speed = 100 rpm, temp = 80 C, mode = p / auto , little vacuum = 800 mbar, to hold the flask. After distilling off nearly all the DCM, suddenly the contents of the flask turns from dark honey colour to creamy milk color and it dries out to a round cake on the bottom. Remove the 1 L DCM, now in the collector flask, and hang that empty flask on again. Now put full vacuum on to remove the last traces of water. Cleaning by 3 x recrystallization: Put MINIMUM quantity of hot (40 C) DRY DCM (or dry 98 +% Ethanol) in the flask until the last remains of the dry stuff dissolves, and add 4 x this DCM-quantity in the form of DRY acetone.
Close with stopper and put 1 hr in freezer. A solid dirty-white crystal mass is formed with a layer of dark red fluid on top of it. Decant the fluid and repeat this step another 2 x and 2 Hrs. You have, the last time, snow white crystals. Dry Weight = 141, 5 gram, close to quantitative yield. You can eventually melt this crystal mass in a alu flat bottom pot on a heater plate at 170 - 175 C.
Then let this melt, VERY SLOWLY, and do not go higher then necessary to melt it, or its starts smoking (you have your first quick-test then: enjoy! ). Cool down to 150 C again, really slowly, 1 degree C per 30 min. (regulate with your temp controller! ), and you got d, l-ICE, after you let it very slowly again cool down to room temperature (with a closed lid on it! , its hygroscopic! ). Advantage: you removed ALL the water in this process! ! ! You can better make the sulfate salt following Logical's method: Let 10 % H 2 SO 4 /Ethanol mix acidifying a 1: 4 mix of freebase Meth/Ethanol. This is not so hygroscopic. Filter and dry the crystals.
So now you know at last how to make ICE cream. Ravers LOVE it! ! ! ! LTEMOTIONSwill always beFREELaBTop. posted 06 - 23 - 99 01: 19 PM Member Yahoo, forgot to tell: Use d-Tartraric acid to get d-Meth! ! ! ! ! ! ! ! 2 Flies in one hit. Ask your beloved moderator, the unforgettable Mr.
SpittartrarBall, he knows how to do that, he recently posted the method, but needs a little explaining for most of you, Im afraid. But thou should NOT be afraid, its easy! (See for a blatant error the Chirality thread in the Serious Chemistry forum). Then you have d-Meth (the softer part) AND l-Meth (which is speedy only). Life becomes easier and easier?
LT/ Sunlight's method of preparing 10 % Methylamine solution in Methanol, from aqueous 40 % Methylamine. This is a convenient adaptation of the Na BH 4 One Pot procedures using aqueous Methylamine instead of the gaseous form. He liberated the Me NH 2 as a gas with dry NaOH pellets: sunlight (Hive Researcher) 07 - 10 - 00 02: 15 If you should try to use directly a 40 % aq. Me NH 2 solution you will get a 60 % yield based on the pure ketone. The procedure to dehydrate (get rid of the water-part) the aq. methylamine is, for example: Put in a 2 -neck flask 700 grams of commercial dry NaOH, and using a compensating pressure separately full attached to one of the necks, add slowly over one hour 350 cc of aq.
methylamine to the NaOH. In the other neck attach a rubber stopper with a teflon tube and to it a glass tube with a gas diffusion (a tiny glas funnel with a glas filter glued in it with 6 seconds glue or two component glue or just melt it tight with a torch), and bubble the MA-gas in 1000 cc of methanol in a flask in a methanol- or water / ice bath. Reaction is endothermic, finally you can heat a bit the NaOH containing flask to force the liberation of the last gas, but its not really necessary, just shake it to see a homogeneous paste. The compensation of pressure can be done using a regular separately full if you attach a 1 -
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