MDMA synthesis via NaBH4 from MDP2P

alquimista00

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hello, i don't know if i did something wrong but i could only get 700ml of mdma free base, and when i was doing the distillation the oil distilled at 275 c,so i'm not sure if what i distilled mdma oil or another substane. ph 6
 

alquimista00

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Hi i got 700ml of mdma freebase. but it destilled at 275c so i'm not sure if what i distilled was mdma oil. the ph is 6 so for crystaliation i need to raise the ph and i would like to know how?? if ou can help me, than you.
 

WillD

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maybe u have unreacted mdp2p or u get -ol variations after mdp2p+NaBH4 react... Alkyl amine variations have a basic pH.
 

hunter12

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can the unreacted mdp2p be reused for another reaction?
 

JustBrowsing223

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Hey there! Some dummy questions.
What does wash down with methanol mean? Just use methanol to wash powder thats sticked to glassware ?
If its stirred for 48h , the temperature needs to be maintained at 8-9 degrees or it can go to room temp?
Whats decent vacuum pump? Sorry, i have no experience with vac. distillation yet.
 

G.Patton

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Hello. Sorry for a long reply.
Yes, it means a rinsing NaBH4 from glassware sides.
8-9 deg have to be maintained for NaBH4 addition. 48h at room temp, correct.
A vacuum pump, which is able to make 0.2-0.4 torr pressure inside distillation apparatus. If you have no experience, I recommend you to learn about distillation. Vacuum distillation apparatus can explode with inappropriate handling. Distillation and distillation systems
Boiling point105 ºC (0.4 torr)
 

spiritveg

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Can I use 39% dimethylamine aqueous solution instead of methylamine gas? If yes then what should be the ratio?
 

Dokodox

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Anybody know if temperatures are highly important or a way to do all in steel so don’t have to import glassware
 

OrgUnikum

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As long you don't get overboard with any part where the reaction is rendered acidic as in PMK to MDP2P and completely refrain from adding any organic acids SS 316 is fine. Treat the parts with hot 75% H3PO4 for some hours for passivation before the first time using them and thats that.

Keeping temperatures low during the reaction is essential, with big vessels I recommend strongly to have some internal coils installed for cooling additionally to the cooling mantle, and get a powerful industrial chiller. But temp control is much easier in metal then in glass, heat-transfer is better in metal by magnitudes.
 

clandestinec

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Video in this synthesis would be nice , only ever done PSE reduction through a distiller and through a few solvents , one question on pmk to mdp2p is it HCl powder or on shelf water solution ????
 

malignoalfa

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If I do not extract with DCM (in my country DCM, TOLUENE and XYLENE are highly controlled), how much would be the approximate loss of yield? Thanks for the answer.

Could hexane, benzene, acetone, or ethanol be used for extraction?
 

malignoalfa

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If I do not extract with DCM (in my country DCM, TOLUENE and XYLENE are highly controlled), how much would be the approximate loss of yield? Thanks for the answer.
 
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