Author Topic: Improved "wet" reductive alkylation help  (Read 11448 times)

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Bandil

  • Guest
Purity of precursors!
« Reply #20 on: July 28, 2004, 12:04:00 AM »
How was the MDP2P made? As it was tinted blue - I assume it was made "wacker style". Wacker MDP2P tends to be quite impure - contaminated with MDP(3/1)P and other strange stuff. So distill it carefully using a short vigreux column.

Do you have an estimate of how pure your ketone is? Impure ketone obviously means more strange contaminants in your final product.

You have also omitted details about how much MDP2P was used in the amination. Try giving a quantitative description of your experiment - this way it's easier to deduce where possible errors might have snuck in  :)

Also - that "fizzing" you get when acidifying. That is only caused by the hydride being destroyed. Unless you have massive amounts of base floating around and the mixture temperature is close to the BP, it wont give rise to any fizzing.

Regards
Bandil


XrLeap

  • Guest
hi Bandil:) MDP2P used with around 60g, to...
« Reply #21 on: July 28, 2004, 12:25:00 AM »
hi Bandil:)

MDP2P used with around 60g, to counter for the impurities present. Yes, it was done from the dirty "wacker" oxidation. Distilled twice uner atm pressure :P , did not improve much.

As for the fizzing, SWIM added the acid in portions, so solution did not turn to acidic immediately, and SWIM turned on the stirrer to stir, trying to get rid of the fizzing. SWIM guesses this has somehow affected the end-product. It was about 1 hour's job to let the fizzing ceased and turned to pH3.

After stripping the IPA, SWIM washed 3 times with toluene. The solution looked slightly yellowish. When NaOH was added to basify, there were some gery sludge formed. Did you have anything like that happened? Are they normal? SWIM will try to filter later, trying his luck to remove them.......


Bandil

  • Guest
MDP2P distillation!
« Reply #22 on: July 28, 2004, 12:44:00 AM »

Distilled twice uner atm pressure, did not improve much.




Bad idea! You'll get massive degradation of you'r MDP2P at the distillation temperature. Aspirator vacuum will suffice - but please do not distill it at atmospherical pressure.

Regards
Bandil




XrLeap

  • Guest
ya, bad idea SWIM reckons.
« Reply #23 on: July 28, 2004, 12:47:00 AM »
ya, bad idea SWIM reckons. SWIM has a decent vaccum pump that pulls safrole at 90C. SWIM has got all his money spent on getting pdcl2 and will need to save up to get a magnetic stirrer.:)


terbium

  • Guest
Anhydrous methylamine freebase.
« Reply #24 on: July 29, 2004, 07:22:00 PM »

ended with 0% yield(molar). The solution always turned dark with fast addition. Anyway, SWIM has not got any yield at all so far,



Geez, wasting all that MDP2P! Why not prepare a solution of anhydrous methylamine freebase in methanol? It is simple to do. Then you could use the standard almost dry method and get 90% conversion of your MDP2P into MDMA.




XrLeap

  • Guest
Thanks fellow bees for all the help:) SWIM...
« Reply #25 on: September 02, 2004, 07:34:00 PM »
Thanks fellow bees for all the help:)

SWIM prepared anhydrous meam in cold methanol, it was weighing to 320g(100g scale dream), and suddenly, it became 290g. SWIM thought about suck back, but didn't notice it.

SWIM went on to add meam.hcl, dissolving all in cold methanol(the same batch), added NaOH to the solution to generate meam gas, on a 250mmol scale. Filtered the salt produced. Water was not removed.

Work up as the article stated, yield was not good, crystal clear solution was obtained after vaccuum distillation. Product tested good with 3 human object. Only problem was that the coming down gave SWIM some fever, as high as 38C(never experienced before in SWIM's 8 years of taking). Some valium helped though.:)