Question I NEED HELP! methcathinone synthesis fail

icebrg1337

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from this tutorial : Synthesis of methcathinone hydrochloride from propiophenone

FIRST STAGE: bromination of propiophenone

50 ml propiophenone mixed with 40 ml hydrobromic acid and 100 ml of distilled water together and stirred for 5 minutes.
60 ml of hydrogen peroxide 35% slowly added in 30 minutes. after all the H2O2 added, stirred for 1 hour and 30 minutes ( temp is controlled on 30C ).
the color turns bright/dark orange.
To the formed bromopropiophenone, 150 ml of DCM added.
solution washed with water ( 2x250ml) then washed with 250ml of sodium carbonate solution.
the color changes to a light yellow.
------------------------------------------------------------------------------
STAGE 2

70 ml of METHYLAMINE 40% is added to the solution ( temp is controlled under 30C ) and stirred for 24 hours.
after 24 hours, the color changes to amber.
The resulting methcathinone is washed with water to remove methylamine.
50 ml of 14% hydrochloric acid is slowly added to the methcathinone solution ( temp is controlled under 30C ) and stirred for 3 hours.

at the end of stage 2, aqueous layer turned to brownish green and after collecting and evaporating it, no crystals.. just some oily smelling shit.

i dont know what mistake i made here... but i think its just the final part.
 

G.Patton

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Hi, have you additionally washed the solution by DCM like in the video?

Have you tried to scratch the oily product by glassrod? It helps to crystallize substance. Your story sounds like there are a lot of side products.

It would be nice if you apply any pic of final stage of crystallization.
 

icebrg1337

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hello and thanks for your reply. yes i did and i think i did not wash the final part well ( methylamine ) and thats why... trying once again right now. ill brb in 5 hours
 

icebrg1337

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god damn.. the bromine vapor is fucking my eyes up ☠️ I can't even take off my mask
 

icebrg1337

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god fucking damn it... the exact same shit. seems like i have to give up on methcathinone :(
 

flusecodns

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The amination process requires an aprotic solvent.
 
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