Author Topic: MDMA a la Os/Bs  (Read 2585 times)

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raffike

  • Guest
MDMA a la Os/Bs
« on: September 15, 2003, 06:59:00 PM »
It's been a while since last pictured writeup so raf thought he'd post one.This one is about reductive amination of MDP-2-P with activated aluminium and methylamine.


Al/Hg a la Os/Brightstar

Ingredients:
 60 grams of very good quality PMK
 30 grams of 0,1 mm Al foil
 95 grams of methylamine.HCl(home-made)
 450 ml of denatured(25% IPA,rest is EtOH) alcohol
 40 grams of NaOH for methylamine liberation
 0,5 grams of HgCl2(reagent grade Fluka)
 50 grams of NaOH for post-rx dilution
 0,5 liters of Xylene

Procedure:
30 grams of aluminium foil(0,1 mm,cut to 2 x 2 cm pieces and slightly folded) and alcohol was added to 3 liter 3-neck RB:

Methylamine.HCl(homemade and little moist from chloroform,raf uses big excess,methylamine is very easily and cheaply made,see Rhodium archive or another picture-essay by raf) in 100 ml water was basified with 40 grams of NaOH in 120 mls of water:

Ketone was pulled out of freezer:

Ketone was dissolved in some 100 mls of ethanol:

Ketone solution was poured to addition funnel.Methylamine solution was poured to reactor along with mercuric chloride:

Overhead stirring was started.Soon aluminium was amalgamted and ketone addition started:

Temp constantly rose(1-2 degrees a minute) and in 30 minutes ketone addition was completed.Temp was kept around 60 C with external water cooling.About 1 hour from start,rx started to calm down and was left to stir another hour.No unreacted aluminium was seen.Whole slurry was poured thru funnel to 5 liter sep funnel and 2 liters of water along with 100 grams of NaOH was added.Solution was washed 3 times with total of 0,5 liters of Xylene and xylene was then washed 3 times with water.Freebase in xylene:

Gassing apparatus(sulfuric acid+hydrochloric acid-->HCl gas,sulfuric acid in addition funnel and hydrochloric in flask) was built from pressure equalized addition funnel and flask.Gassing tube is PTFE.Freebase is constantly stirred with magnetic stirring.



Freebase after gassing:



Product after purification:

Yield 42.8 grams(that cup weighs exactly 3 grams):



raffike

  • Guest
Ras has never got into very high yields like...
« Reply #1 on: September 15, 2003, 07:15:00 PM »
Ras has never got into very high yields like 90% w/w.Raf usually gets constant 70-80 % w/w(highest so far has been 46 grams from 60 gr of ketone) has been achieved and quality has always been excellent.Reduction with activated aluminium offers very little room for mistakes but raf likes it cuz it's quite easy,gives constant yields and one reduction takes only about 3 hours from start to complete(raf has ran 4 60 gram PMK rx's in one day without problems).


hypo

  • Guest
question
« Reply #2 on: September 15, 2003, 07:34:00 PM »
any reason you don't distill your freebase?
i see no reason why for example the reduced condensation product
of MDMA and MDP2P would not be in your product.

ps: i think this is a fraction cutter, not an addition funnel.  ;)


raffike

  • Guest
any reason you don't distill your freebase?
« Reply #3 on: September 15, 2003, 08:14:00 PM »
any reason you don't distill your freebase?
That xylene/freebase solution looks dirty i agree.
Raf doesn't have a pump at the moment,that ketone wasn't made by raf also but by a friend of raf.Raf recrystallizes his product which should give purity comparable with a purity seen with distilled product.IPA/ether rxtal works,but acetonitrile should work better.Careful rxtal is easier to do than distilling(isolation of freebase from post rx mixture is a bit difficult).Rxtal should give product of a very good quality.


hypo

  • Guest
isolation
« Reply #4 on: September 15, 2003, 09:01:00 PM »
> isolation of freebase from post rx mixture is a bit difficult

have you tried filtering through celite (=diatomaceous earth, kieselgur)
after basification? works like a charm. when clogged, just scrap the
surface until you can see the white celite layer.

then you can for example evap the alcohol, separate the freebase,
take up in dil. HCl and continue with the usual A/B.

must read on the subject:

Post 384725

(Chromic: "Celite", Methods Discourse)



Rhodium

  • Guest
Recrystallization is NOTsufficient
« Reply #5 on: September 15, 2003, 09:08:00 PM »
Raf recrystallizes his product which should give purity comparable with a purity seen with distilled product.

No, that is incorrect. If it was that easy, then no professional chemists would go though that trouble when purifying their products, and the literature is scarce with procedures where only recrystallization of an amine salt is used after such a "crude" method of preparation as reductive amination. Sometimes when a simple reduction of a nitro or azide group has been performed, the product is pure enough for A/B extraction and recrystallization to suffice, but not reductive amination.

RoundBottom

  • Guest
gas drying?
« Reply #6 on: September 15, 2003, 10:02:00 PM »
if you are using H2SO4 and HCl, how do you dry your gas from the generator?  does that PP tube have some dri-rite in there?  the only time you might not need a drier is if you are using H2SO4 and NaCl (salt).

other than that, good job... love the ghetto rig.


raffike

  • Guest
Raf usually doesn't dry his HCl gas,he used to
« Reply #7 on: September 15, 2003, 10:11:00 PM »
Raf usually doesn't dry his HCl gas,he used to but that drying doesn't seem to be needed,there is very little if any H2O carried over.Getting solution,that is to be gassed,dry seems to be much more importnant.Another problem one might face is over-gassing.There's an easy way to stop at right moment.One must keep an eye on freebase/NP solution and if one sees that solution starts to turn darker where gas bubbles enter liquid,one must stop and throw beaker into freezer.Over-gassing discolours product and renders it more impure.


Rhodium

  • Guest
Drying HCl gas with sulfuric acid
« Reply #8 on: September 16, 2003, 02:06:00 AM »
If you are using H2SO4 and HCl, how do you dry your gas from the generator?

An excellent way of drying HCl gas involves bubbling it through an inch or two of conc. sulfuric acid in a gas wash bottle (or equivalent contraption):


MisterWize

  • Guest
Nice one Raffike
« Reply #9 on: September 16, 2003, 04:14:00 AM »
Cheers for that Raff,
                      Its nice to see how ppls labs look and to see the stages in picture rather than just descriptions.  Also good to see the colours at each stage.

But beeware of LE getting hold of that camera, there must be some incriminating pictures stored in your camera by now.

So what is next picture synth that you are gonna put up on here Raff?

abolt

  • Guest
Nice post Raf
« Reply #10 on: September 16, 2003, 05:40:00 AM »
Follow the chiefs advice about the gassing bottles. ;)

Post 443917

(abolt: "Cool info, Buster", Chemicals & Equipment)


As your pump is not working.............can I assume that the reason you are not getting a gram for gram yield is due to undistilled p2p?


raffike

  • Guest
But beeware of LE getting hold of that camera,
« Reply #11 on: September 16, 2003, 05:44:00 AM »
But beeware of LE getting hold of that camera, there must be some incriminating pictures stored in your camera by now.
Raf keeps nothing in his camera and his computer is also clean.He has these stored on a cd should they be needed again.
So what is next picture synth that you are gonna put up on here Raff?
Probably MDA via oxime reduced by activated aluminium.Hydroxylamine has been already ordered and should arrive in few weeks.
Rhodium,i will mail you these pics as soon as possible. :)


technology

  • Guest
Much compliments
« Reply #12 on: September 17, 2003, 04:26:00 AM »
much thanx.. going out to raffike.. this is a great posts that all bees will greatly appreiciate..

keep up the good work..'

peace.

TECK

scram

  • Guest
Not to complain raffike but your wasting ...
« Reply #13 on: September 18, 2003, 04:07:00 AM »
About gassing: You could used the H2S04 thrown into Sea salt in the garden sprayer. If you want to be sure its anhydrous then attach the little 120ml oil resavoir which comes with the MidiVac pump inline between sprayer and wand/nozzle. Pack the 120ml with drying agent. You then easily control pressure by the hand pumping of sprayer and volume of the gas by the wand.

Not to complain raffike but your wasting precious methylamine and most likely losing a significant amount of product due to the excess al. 30-35g al per mole ketone works just as well as your 90g al used above per mole. Seriously, regarding the MeAm, using reagent grad 40% methylamine, a 2/1 (amine/ketone) ratio is plenty. It's been noticed several times that using too much MeAm seemed to consistantly REDUCE yield; especially at your 4.25 molar excess. Cut that in half next time along with your Al and see if you get better results. I can only comment these observations based on HD foil measuring 0.03mm thick.

Regarding:
"Methylamine solution was poured to reactor along with mercuric chloride:"

Are you saying you threw the MeAm in at the exact same time you put the Hg in? If so explain, because I've noticed throwing the MeAm or ketone in ceases further amalgamation.

....This nigga be tricken'