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-

