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Post NaBH4 crystalization problems

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b00ked:
I just ran my first NabH4 reduction on MDP2P. I generated the 10%MeAm in MeOH solution in situ by dissolving 70g MeAm.HCl in 500ml methanol then adding 42g NaOH slowly under stirring and cooling. This took roughly 2 hours as I had to periodically put the solution into the freezer. When this step was completed I filtered off the NaCl. This was my first time working with MeAm and I was unsure if the step worked but the MeOH absolutely stunk like MeAm generated from the Nitromethane Al/Hg. To this 100g of -15C MDP2P from a performic was added and allowed to stir for 30min. Under cooling 10gms of NaBH4 was added in 2g portion over 5 hours. The solutin turned from a orange clear to a milky pink/red color. I allowed to stir for 20hrs slowly warming to room tempeature. Post reaction was basified with 4L 5% NaOH solution and freebase was seperated. It was pink/brown color. Freebase was dissolved in 500ml acetone and 100ml 50% HCl was added. I was expecting the MDMA.HCL to precipitate however nothing happened. The whole solution is in the freezer cooling right now to see if anything happens. Did I screw up? I thought you could crash the crystals out of solution this way. The solution did not warm up too much upon addition. Any ideas?

b00ked:
yield freebase was 78g MDMA x 1mol/192.7 g = 0.4 mol MDMA
started with 100g MDP2P x 1mol/178g = 0.56 mol MDP2P

% yield MDMA = 0.4 mol MDMA/0.56 mol M2P2P = 72.3% MDMA feebase

psytech:
You have a solution of mdma hcl, acetone and h2o, distill of the acetone h2o azetrope the slow distill off the water check you ph for 6 or 7. That should work

cublium:
The solutin turned from a orange clear to a milky pink/red color
Usually turn bit lighter during the addition of boro
Post reaction was basified with 4L 5% NaOH solution and freebase was seperated. It was pink/brown color.
You should've at least AB'd it,especially if freebase didn't seem pure and pink doesn't seem like pure to.Cub always got bright yellow or almost white freebase even before AB and after AB it looked like water,smelled kind of fishy though not overwhelming and not ketone like.It smelled bit like ammonia but smell was weak and definitely distinguishable from ammonia,it smelled like...freebase :)
Freebase was dissolved in 500ml acetone and 100ml 50% HCl was added.
Mhmh??
Should have gassed.Anyway just evap and see what remains.

XrLeap:
Hi b00ked,

The method that you used looked ok to SWIM. However, you did not indicate the temperature of the solution while adding NaBH4. As per Sir Labtop, the best is from 0-5C.

SWIM always perform an A/B extraction to pull all freebase from the methanol solution, and to seperate what is not needed.

SWIM also always try to distill his freebase to a clear color oil, this way, salt/.HCl can be obtained using any preferred method.

Cheers,
XrLeap

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