Author Topic: Reductive Amination  (Read 495 times)

bizzybees

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Reductive Amination
« on: August 27, 2012, 03:58:39 AM »
Ref Doctor Gonzo / Methyl Man method.

Reaction contents gets poured in beaker.
Add 700mL Water and 262g of NaOH
Stir
Add 500mL toluene

Now Seperate.

The Dr suggests toluene or xylene.

Could DCM be used as an alternative to either toluene or xylene?

Electro´S

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Re: Reductive Amination
« Reply #1 on: August 27, 2012, 04:30:16 AM »
With MDMA i don´t know, but Meth HCl disolve completly in DCM  :o.
May be not.
Hexane is Fine but all must be cold before add the solvent.

carl_nnabis

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Re: Reductive Amination
« Reply #2 on: August 27, 2012, 04:53:06 AM »
I wouldnt use DCM theres just too much crap it would dissolve, but neither would i use xylene but for other reasons.
Use some ether (has some advantages) or hexane (better cause doesnt dissolve so much water) instead maybe?
"It's like the drug trip I saw when I was on that drug trip!"

bizzybees

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Re: Reductive Amination
« Reply #3 on: August 27, 2012, 08:49:00 AM »
Comments appreciated and duly noted  ;) thank you

POSEIDON

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Re: Reductive Amination
« Reply #4 on: August 27, 2012, 03:44:28 PM »
Look this pdf
The chemists are a strange class of mortals, impelled by an almost insane impulse to seek their pleasures amid smoke and vapour, soot and flame, poisons and poverty; yet among all these evils I seem to live so sweetly that may I die if I were to change places with the Persian king.
— Johann Joachim

bizzybees

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Re: Reductive Amination
« Reply #5 on: August 29, 2012, 12:17:26 AM »
Looked at the pdf.

Are you saying toluene would be best?

"The mixture was refluxed for 2 h.
After cooling to room temperature, an 8.3 M NaOH solution (16.0
mL, 0.13 mmol) was slowly added, and the crude methamphetamine
base extracted with toluene (3 × 20 mL). The combined
organic layers were dried over MgSO4, and the volatiles removed
in vacuo to reveal the crude methamphetamine base as a brown
oil."


lugh

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Re: Reductive Amination
« Reply #6 on: August 29, 2012, 01:07:12 AM »
Any non polar solvent will extract the free base, but of course some work better than others  ;)  There are numerous techniques for isolating free bases which can be found using the search engines here and elsewhere, there's no good reason to make things too easy for newbees for reasons that can be found in this thread:

https://the-collective.ws/forum/index.php?topic=9679.0

as far as your question, both toluene and xylene will work quite well  :-X You need to do a lot more reading before proceeding, the end results from the effort applied 8)
« Last Edit: August 29, 2012, 01:55:55 AM by lugh »
Chemistry is our Covalent Bond

bizzybees

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Re: Reductive Amination
« Reply #7 on: August 29, 2012, 09:05:10 AM »
Really useful info. ty..

From one of the links on there im reading this which I have read before.

http://www.erowid.org/archive/rhodium/chemistry/mdma.impurity.study.html

I have been confused by this write up more than any of the others.

Majority of papers I read some way or another always lead to MD-P2P. Then the conversion of this to MDMA hence my original question.

With the particular paper mentioned they talk about MD-PBP (note the B not P) and also PMK

PMK confuses me cause some say its actually (MD-P2P.) some say its a new way of getting to MDMA. Im also confused if this paper has typoed MD-P2P for MD-PBP
« Last Edit: September 01, 2012, 09:50:56 AM by bizzybees »

fractal

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Re: Reductive Amination
« Reply #8 on: September 03, 2012, 01:15:17 AM »
No PMK is MDP-2-P, it stands for piperonyl methyl ketone. MDPBP is a completely different unrelated drug (3',4'-Methylenedioxy-?-pyrrolidinobutyrophenone).

letters

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Re: Reductive Amination
« Reply #9 on: September 04, 2012, 10:38:58 PM »
What Lugh said.
 Most non polar solvents will be ok for extracting freebase. DCM also. Toluene, along with diethyl ether are always my preferred freebase extraction solvents. Toluene beacuse it has good solvating power and is "self drying" (azeotropic distillation) and Et2O because of its solvating power and its low b.p.
I usually refrain from DCM in extractions if I can because of its tendency to create emulsions.

Sedit

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Re: Reductive Amination
« Reply #10 on: September 04, 2012, 11:22:37 PM »
We do have a short question thread and after returning from a short hiatus it seems that most people that frequent the forum now don't know this since they are all cluttering up the forum with threads that can be answered with a simple yes or no....

Shape up people sheesh  ???
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sassa

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Re: Reductive Amination
« Reply #11 on: September 06, 2012, 11:31:00 PM »
But he is talking about reductive amination Al/Hg i think...if one try to extract the reaction mix with DCM here will fail almost sure,or will be a painfull workout...it will finish with a freak  emulsion sure,...because all that crap,powdered alumminium,...will tend to sink to the bottom with the DCM,so clean it afterwards will be a pain.
   Yeah too,the mix resulting from Al/HG reduction have way more density than water alone,it´s a thick mass...and on that situations,i allways got a freaking emulsion using DCM as extracting solvent.,..that works fine only extracting on light acid solutions ,like the one resulting on the benzo wacker.So if you can´t use toluene or xylene,use anything that will go up on the separation,You can allways experiment with few ml of final mix reaction and test extracting  with DCM to see how it works,but sure use DCM here must be the last alternative i think.
   DCM good for Benzowacker,but not at all on the AL/HG.
  I worked  a lot Al/Hg both with Xylene(on the begining) and Toluene,and are exactly the same.Pick up the one it´s easier and cheaper to get...Anyway,both will work fine without emulsions if you only stirr the mix carefully long time without big hard shaking.
  Seems xylene tends to not separate so quickly,it mixs  better with the reaction mix,so possibly extracction can be more efficient,but nothing that you can´t do extracting with toulene with pacient....Like said,i prefer toluene because avalibility,price(way less than xylene) and easy work...Allways a 5 litre bottle on room´s corner it´s a must,...you can extract with it almost every reaction we talk about,and re-use after extracted the goods and clean it with water washes....I used to have labelled recicled toluene as "benzo recicled" and "al/hg recicled" , and use each bottle to extract each reaction.. When i think i used it too much,...i bought another 5 liter bottle cheap as hell and have toluene for months.Too,i used to let alone big amounts of used toluene distilling along an afternoom when not to much to do, to get liters of almost fresh again toluene to use....only reserve it, and distill all on one run.
   I only used DCM to extract acid solutions,and on that situations,worked fine allways....When density of mix it´s only little bigger than plain water,then begins problems with DCM.
« Last Edit: September 06, 2012, 11:37:39 PM by sassa »

Sedit

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Re: Reductive Amination
« Reply #12 on: September 10, 2012, 12:49:04 AM »
Yes you never EVER use DCM to extract Na cation containing solutions as a horrible emulsion will form. Im sure this sule applys for all alkali cations.
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no_dream

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Re: Reductive Amination
« Reply #13 on: October 10, 2012, 05:52:14 PM »
DCM is very prone to create emulsions, impossible to separate. Ether is much better, but the solubility in water is too large.


Whale

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Re: Reductive Amination
« Reply #14 on: January 22, 2013, 09:01:04 PM »
As said above DCM doesnt work that well and ik if you cant source toulene then you can always get xylene at the big orange store ;)