Author Topic: Formyl MDA, and crystallization  (Read 1947 times)

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grellobanans

  • Guest
Formyl MDA, and crystallization
« on: June 06, 2003, 03:54:00 AM »
Swim is wondering about the chemistry behind this part of the leuckart. Some writeups hydrolyze with HCl, others use KOH. What is happening here that allows you to use one or the other? If HCl is used, is a salt solution formed? And if KOH is used, is the freebase formed?

Another question is MDA crystallization. Does it form hydrates like MDMA? And how necessary is gassing, since some writeups just distill and the crystals spontaneously form (?).

Rhodium

  • Guest
mda leuckart
« Reply #1 on: June 07, 2003, 07:42:00 AM »
Some writeups hydrolyze with HCl, others use KOH. What is happening here that allows you to use one or the other?

Formyl-MDA is an amide, and amides can be hydrolyzed to the free amines either with acid or with base - your choice.

If HCl is used, is a salt solution formed? And if KOH is used, is the freebase formed?

Yes. Yes.

And how necessary is gassing, since some writeups just distill and the crystals spontaneously form (?)

Oh yeah? Point me to such a writeup, please.

grellobanans

  • Guest
Unclear Writeup
« Reply #2 on: June 08, 2003, 06:51:00 PM »

https://www.thevespiary.org/rhodium/Rhodium/chemistry/mdp2p.leuckart.txt



"Add 23g 3,4-methylenedioxyphenylacetone to 65g HCONH2 (formamide)
      and heat at 190 deg for five hours.  Cool, add 100ml H20, extract with
      C6H6 (benzene) and evaporate in vacuum the extract.  Add 8ml MeOH
      (methyl alcohol -- methanol) and 75ml 15% HCl to residue, heat on
      water bath two hours and extract in vacuum (or basify with KOH and
      extract the oil with benzene and dry, evaporate in vacuum) to get
      11.7 g 3,4-methylenedioxyamphetamine (MDA)."

This person just evaporates the extract in vacuum and gets 11.7g? Swim thought that was weird from the start.

raffike

  • Guest
That's MDA as base
« Reply #3 on: June 08, 2003, 06:53:00 PM »
That's MDA as base


madprosr

  • Guest
i think KOH works better
« Reply #4 on: June 11, 2003, 02:00:00 AM »
swim didn't get either hydrolysis to work, but HCl seemed to destroy things much more quickly.

grellobanans

  • Guest
HCl
« Reply #5 on: June 11, 2003, 02:38:00 AM »
What concentration of HCl was used? And for how long?

FlyBoy

  • Guest
If you had say...
« Reply #6 on: July 29, 2003, 11:21:00 PM »
If you had say 100ml of rxn mixture at the formyl amide stage you would pour it into a 500ml RBF with some boiling chips and add 200ml of 28% HCl.
I read, muriatic works just fine for hydrolyzation.

grellobanans

  • Guest
Crystallization
« Reply #7 on: August 05, 2003, 07:00:00 AM »
No one has answered the question of "does mda form hydrates?" yet. Does it? Swim is contemplating various methods of crystallization that don't involve gassing.

Aurelius

  • Guest
Citrates and Tartrates
« Reply #8 on: August 05, 2003, 07:03:00 AM »
dissolve some citric or tartaric acid in a non-polar, add your non-polar solution of MDA (or other freebase amine) dropwise and you'll get the crystals you want.  obviously, they're not hydrochlorides, but it keeps you from having to gas anything.


grellobanans

  • Guest
Without a pH meter
« Reply #9 on: August 05, 2003, 07:56:00 AM »
sorry, no citric or tartaric acid available.

If swim had no pH meter, is a/b crystallization and sulfate salt formation tricky and too difficult? swim can gas if it is absolutely the last choice. gassing is just not that great without a fumehood.

"Take dcm/mda freebase and chill in freezer for several hours.  Put in a big ass beaker with a stirbar and put it on a stirrer.  Begin heavy stirring and add muriatic.  SWAM never measured or did ph here...just added and watched until a snowstorm started in the beaker...Stir for about another 1/2 hour and put back in freezer for another few hours...filter off goodies...You should get a majority of your xtals the first time...if not add a bit more muriatic and see if any more xtals appear...if not, add 2x acetone and freeze again...Note: these xtals will smell heavily of HCL, and for SWAM they started turning brown after a month or so" -Post No 107190

Found this, but this guy's crystals turned bad. Is this method good? Will the crystals be fine if distilled freebase is used and recrystallization? And also, what solvent is best for mda recrystallization? IPA like mdma?

Aurelius

  • Guest
citric and tartaric acids
« Reply #10 on: August 05, 2003, 08:17:00 PM »
NOT AVAILABLE?!?!

Does anybody visit their grocery store anymore?


grellobanans

  • Guest
How?
« Reply #11 on: August 06, 2003, 01:41:00 AM »
Cream of tartar - "potassium hydrogen tartrate, KC4H5O6, the acidic potassium salt of tartaric acid. It is used as the leavening agent in baking powders."
How would one convert that into a usable acidic form?

Citric acid - what are people supposed to do, extract it from lemon juice? that's pretty silly, like extracting tryptophan from milk or something

Edit: swim UTFSE and
the procedures are pretty drawn out and seem like a waste of time for someone who has other acids right on hand

Aurelius

  • Guest
Silly
« Reply #12 on: August 06, 2003, 03:50:00 AM »
Well, I was giving you options for avoiding gassing.  Those were the best 'quick' answers I could give at the time.  Perhaps you should consider your use of the term 'silly'.  I think that instead of 'silly' the term 'lazy' comes to mind.  Just gas the stuff.  IT IS NOT HARD.  Not to mention you can be tartaric acid and citric acid in their pure forms from several OTC suppliers. 

the tartrate salt you speak of can be dissolved in conc. HCl acid and stirred for a while.  Then extract the tartaric acid and evaporate to leave it as the crude acid.  ( you only really need the crude acid)


grellobanans

  • Guest
Silly -> Inefficient
« Reply #13 on: August 06, 2003, 06:22:00 AM »
silly was perhaps not the right word. Inefficient? In terms of the amount of starting product needed and the end yield (gallons of lemon juice). If there was no other way, then it would be fine, but there are other ways that are just as fine with less effort. For example, there's 2 different procedures for the synth of oreos. One is 2 steps long, the other is 10. Plus, you have all the materials needed for the 2 step one. Why bother with the 10 steps?

Anyway thanks for your suggestions. After thinking, swim is probably going to gas. It really isn't that hard to do, it's just that even with a fan, the fumes get irritating. maybe swim has become sensitized after all this time?