Subject: QUIZ:Meth via chlorephedrine int..pop-i My anonymous Net Pal asked me to post this for information purposes only. -oLIVEoIL This synth has been handed down to me through some fairly scandalous routes... It was badly typewritten on chemStained paper, and judging from the spelling, did not come from the library... This is my interpretation of it...alot of guesswork (fr instance: Step Two was originally written as follows "now boil it in alchohol. When it turns red, then put in some ether to make the crystals come back") What follows is my best guess as to what it all means, I have fleshed out the hydrogenation, PHing and crystallization sections, since I have some experience there, but that doesn't mean they're accurate. I don't have very good University library access right now, even so, I have trouble interpreting chemical literature, my vocabulary and background are lacking and I have no immediate backtoSchool option, so I'm asking for some help. I do know, for a fact that some real potent crank is produced via this method, if done right. Judging from the output of some of the more prolific contributors to this Newsgroup, they have better things to do than arduously type me through a complex synth like an underpaid cyberBabysitter, for this reason I have formatted this post multiple choice, to facilitate responces by reducing to Cut and Paste functions....but feel free to tear into it in any manner you see fit...If your're just guessing, like me, please extend me/us the courtesy of copping to it, but all responces are appreciated. For those of you who DO have University access, here are some references....I haven't seen them yet, so I don't know how closely they apply, I/we would appreciate your posting any pertinant info you may obtain from the literature. Reduction of Pseudoephedrine or Ephedrine: Emde, Helv.Chim. Acta 12, 365 (1929) O.Y.Magidson & G.A. Garusha, J. Gen. Chem. (USSR),11, 339 (1949) Preparation of Four Phenylpropylamines by Catalytic Hydrogenation Hartung & Munch, J.Am Chem Soc. 53,1875(1931) Allen, AC, and Kiser, WO. Methamphetamine from ephedrine: I. chlorephedrines and aziridines. _J F S_. 32:953-962. (1987). *SPECIAL DISCLAIMER* If you have read to this point, you should know better than to try and use this as a procedure. If you skipped anything, maybe you should go back and read it. If you are interested as to whether or not this is viable, then follow the thread (if there is one)...these are questions, not answers. *standard disclaimer* It should be obvious that I am not a chemist. Merely a chemHacker experienced in certain chemical processes/techniques. This is not one of them. This is not intended as a procedure. All responses expounding ethical and/or moral pretences will be mutilated for entertainment purposes and your addressing circulated amongst low-life scooter-trash. This describes illegal activity, this is posted cross-eyed and double blind anonymous, I could be making this up, I have already been publicly denounced, don't try this in Tupperware... I have hereby disclaimed, you have been warned....be careful in realTime, remember to keep your mouth shut. *disclaimer over* I WILL RE POST THIS SYNTH IF IT ACHIEVES PRAGMATIC EMPIRICISM STEP ONE Place a 5L flat bottomed flask or vessel capable of fitting a condenser on a magnetic stir plate, then add 0.41 kilos(1 lb) L ephedrine, and: (1) a) 1.2 Kilos ( 0.75 Ls) thionyl chloride (SOCl2) b) ____ Ls thionyl chloride (SOCl2) c) ____ Ls thionyl chloride (SOCl2) and _____________ into flask, being careful to assure adequate ventillation of the exhaust, SOCl2 fumes are suffocating, reaction is hypothermic. Fit a condenser to the vessel and run it at very cold temperatures using ethanol or the like as a coolant. Once again, the condenser must be externally vented, taking care that no back pressure is created. Leave the stir plate set at a low RPM and use a big stir bar, so as not to induce too violent a reaction. It will take up to an hour for all the l-Ephedrine to dissolve. After it has done so, let react for another hour, then add 1L chilled diethyl ether, transfer flask to ice bath. Do not disturb 1 hr. Precipitation should occur. Filter, discard the filtrate & rinse the crystals with more chilled ether, vaccuum dry . The yield after recrystallization of this intermediate should be equal to the mass of the l-Ephedrine precursor. (2) The first step in this process as described is a) accurate b) not quite right. Here's why... c) OK, but you forgot to ... d) an indication that any endeaver in this direction shoud be abandone= d STEP TWO In a 5L boiling flask, the chlorephedrine intermediate is added to (3) a)1.25 Ls methanol b)________ Ls Methanol c)________ Ls Methanol & ________ d)________ Ls __________ e)other... and gently refluxed for 1 hour, The solution should turn to a deep burgundy color. Now strip volatiles 'in vacueo'. (4) True/False: Carefully boiling/distilling off volatiles will work if no vaccuum is available. When boiling has ceased at 110=BA C go to next step. Now add 1L chilled diethyl ether, place flask in ice bath, chlorephedrine intermediate should precipitate once again. The crystals are filtered out. The yield after recrystallization of this intermediate should be equal to the mass of the l-Ephedrine precursor. (5) The second step described here is a) accurate b) not quite right. Here's why... c) OK, but you forgot to ... d) totally wrong, try this instead... e) unnecessary STEP THREE hydrogenation In a large beaker make an amalgam of (6) a) 50 gms 10% palladium on carbon b) ___ gms 10% palladium on carbon c) ___ gms 10% palladium on carbon or ________ d) other _______ and enough Hexane to moisten. Measure 1.25Ls of methanol, set one quarter of it aside, add remaining methanol and chlorephedrine intermediate to beaker w/ amalgam, stir, then transfer the contents to a pressure vessel. Now use the remaining alchohol to rinse any residue remaining and add. Seal the pressure vessel and attach it to a shaker. Purge it 3 times with 40psi Hydrogen gas then pressurize to 40-60 psi and start shaker. Repressurize whenever psi falls below 20lbs. Continue until the pressure no longer falls, between 0.5 to 2 hours. Let stand another hour before releasing pressure through an aspirator into a safe exhaust. Combine contents of aspirator and pressure container into a glass vessel which can be stoppered. Rinse containers with methanol and add. The holding vessel should then be filled to the top with methanol to purge the air and prevent any wierd oxidation catastrophes, then stoppered. Let sit for a few hours until Pd/C settles out. Carefully suction out the reaction mixture without disturbing Pd/C sedimentation. To increase yield, refill container with methanol and repeat last step. Now, filter solution until it is free of catalyst, adding more methanol to carry solution through filtercake as necessary, solution of oil/methanol is orange colored when clean. Now strip methanol from oil 'in vaceuo'. (7) In this case, the hydrogenation process: a) works fine with Methanol as a solvent b) works better if ________________ is substituted for methanol. (8) The hydrogenation step in this process, as described, is a) accurate b) not quite right. Here's why... c) OK, but you forgot to ... d) lethal (9) True/False: Carefully boiling/distilling off volatiles will work if no vaccuum is available. When boiling has ceased at 110=BA C go to next step. STEP 4: PH and crystallization Prepare crytallizing medium: Add diethyl ether to two 1 gallon glass jugs till 3/4 full, lubricate stoppers with vaseline and seal, pack with dry ice and rock salt in an ice chest. Test PH, if between 5.0 and 6.6 go to crys. step if alkaline, gas with anhydrous HCl, until 6.0, then go to crys. s= tep. if acidic (under 4.5), freebase with lye solution and sep funnel to about 12, titrate with HCl acid to about 8, concentrate in vacueo, or heat to 110=BA C until boiling ceases. Test PH again: if greater than 9 -> repeat titration and drying step= s if between 5.0 and 6.6-> go to crys. step between 6.7 and 9 -> do 'if alkaline' step above (10) The PH step as described above: a) Will work b) Will work better if _______ c) Should be abandoned in favor of _______ d) Is a pretty expensive way to produce sodium chloride Crystallization and consumption: Quickly add anhydrous oil to the cold ether, fill jugs to top with more ether, stopper and keep them as cold as you can, crystallization may be immediate or take a few days. Either way, crytals may continue to form for up to two weeks. Switch to regular ice and rock salt after dry ice evaporates. Never put ether medium in the freezer because fumes can be ignited by sparking relay or compressor motor which will result in rapid dekitchenation. =46ilter,wash crystals with cold acetone, test on neighbor's pet ,slam. Any discussion of synthesizing Methamphetamine from ephedrine would be incomplete without beating the old pseudo vs L-ephedrine horse. 11) This procedure, if performed correctly: a) produces nice d-meth from L-ephedrine and nasty, crampy, skull-gnawing L-meth from pseudoephedrine b) produces nice d-meth from pseudoephedrine and a wierd drug from L-ephedrine c) produces the largest percentage of nice d-Meth in racemic product from L-ephedrine d) produces the largest percentage of nice d-Meth in racemic product from pseudoephedrine f) produces racemic Meth from L-ephedrine only g) produces racemic Meth from pseudoephedrine only h) produces racemic Meth from either i) produces nice d-Meth from either j) produces sudden death in neighborhood pets e) other... *final disclaimer* I am not 'in the business', I have grown weary of 'the business' and worrying about the cops. It is interesting to note that the existence of one is very much dependent upon the health of the other. You would do good to avoid both. If you think about it, that is where the real value of this Newsgroup lies. -POPEYE-