Set this solution aside.
5. Combine the 25g MDP-2-P, 20mL MeNO2, and 50mL MeOH and pour them into the addition/sep funnel.
Rinse your beaker (or whatever you used) with a tiny bit of additional MeOH to get the residual ketone and
add it to this MDP-2-P/MeNO2/MeOH solution.
6. Very slowly and carefully (w/gloves, glasses, long sleeves and a Hail Mary if you’re Catholic), using a large
funnel, pour the HgCl2/MeOH 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 MeOH 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 MeOH. This is the magic moment when
you want to begin dripping in your MDP-2-P/MeNO2/MeOH 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/nitromethane 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. A’s trial and error regarding this reaction’s parameters.
If you used the kind of foil specified, prepared it as specified, used no more than the specified 400mg HgCl2,
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.
I’ve seen this reaction get out of hand in a 1000mL flask, and it isn’t 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 MeOH dripping
really fast down out of the condenser. I know it’s hard to believe, but this is what you want, this is good.
I’m 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 won’t want to speed it up much. The concept
here is that you want the addition of the ketone/nitromethane 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. It’s tricky, and imprecise, but with a little experience and intuition you’ll 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, don’t cry to me. The addition should take about 40-45 minutes in total, and as
it’s 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
20-30mL of MeOH 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 HgCl2, where a dark metallic gray with definite green overtones (from
unreacted 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 so—very 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 nitromethane. Mr. A was
never successful in using thicker aluminum, and doesn’t want to be! Why would someone want to make a
reaction take any more time than it needs? Beats me! I’m mystified! The approach illustrated in this writeup
optimizes this reaction to finish in 3 hours 45 minutes from beginning to end, and it probably doesn’t 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 H2O + 262.5g NaOH) and let it cool to room temp or below (safety glasses!).
15. Into a separatory funnel no smaller than 2000mL 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 MeOH 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 MeOH and add it to the funnel also.
16. Slowly pour the NaOH solution into the sep funnel (gloves and glasses! no excuses!). That’s right, don’t
dump it in wholesale. Basifying should be a gentle process. If you bully those molecules they may decide
they’re 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 400mL toluene followed by
once with 100mL 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 don’t 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 it’s 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
that’s 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 haven’t 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 500mL H2O and a final time
with 500mL of a saturated NaCl solution to remove any traces of solvated HgCl2.
20. Dry your toluene/product solution with 30g of your favorite drying agent (MgSO4 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 muriatic
(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 20-21.5g raw odoriferous product that will purify via careful recrystallization
to 17-18g of beautiful snow-white MDMA! Ain’t life grand?
~~~”There’s a methyl to my madness”~~~
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WISDOMwillWIN
Re: DETAILED METHODS for NON-CHEMISTS
P2P–* METHAMPHETAMINE, racemic mix. :
———————————————————————————————————
Materials :
See MDMA, Isosafrole etc.
———————————————————————————————————
Chemicals :
See MDMA, exept :
Change MDP2P to P2P, Phenyl-2-propanone.
Method :
The original link is broken, or the file is deleted, so:
LaBTop ………. posted 06-23-99 01:04 PM
Member
Making of d,l-Meth (Ice) .
Ingredients:
? 138 gram P2P = +/- 1 grammole.
? 1000 ml Methanol (+ 10 % weight Methylaminegas dissolved in it = +/- 100 gram)= +/-3gmol.
? 36 gram MgSO4.7H2O , magnesiumsulfate (dry at 300 C for 2 Hrs in oven to get MgSO4.1H2O)= 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 attrack 2 gmol H2O, during imine forming.
? 15 gram NaBH4 as a reducing agent for the formed (waterfree !) 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 MgSO4 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 MgSO4. Let stand and wait till all the
MgSO4 is on the bottom. Now quickly tap off the now DRY MeOH/MA mix in a 2L 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 2L flask and close again. Keep 2L flask in Silicone-oil bath at 20 C.
Silicone-oil only slowly warms up! Do not apply heat now, it’s only meant as a cooling medium in this stage.
Now add SLOWLY via a dropping funnel the 138 gr P2P to the 2L flask under strong mixing. The temperature rises to 23 C during the (waterfree) 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 reactionmix 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 2L glas erlenmeyer with flat bottom and add a mixbar. 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 2L erlenmeyer. Now put the 2L erlenmeier on magn.mixer, in a icecubes/methanol bath (-10 C) and start strong mixing. Put a Funnel on top of 2L erlenmeier, in rubber ring. Now start adding, every 5 min., a teaspoonfull (flat off!) of boro and wash in with
minimum methanol. After every spoonfull, 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, do’nt 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 waterpart with an aspirator + siliconetube.
Fill the rest (water+DCM+oil) in a seperator funnel and tap off only the DCM+oil = 550 ml.
(DCM boiling point=40 C).
The leftover MgSO4 and boro salts stayed nicely in the waterpart.