I would like to make MMC in NMP. The problem is that I don't have pH paper. How problematic is it if I over-acidify at the end? Or could you tell me how much 30% hydrochloric acid I should add at the end when using 100g of 2b4m? I'm acidifying in DCM+water.
Mephedrone synthesis (4-MMC) in NMP solvent. Large scale.
If you buy electric, do yourself a favor by spending extra to get a glas probe. Otherwise it will dissolve (yes, been there)
Why to use Benzene and NMP. Use Ethyl Acetate instead. Much safer. Change the mono methyl amine aqua for alcohol based.
After adding water. Separate layers. Take the “oil” layer and distill the EA off. Fatter this step. Cool down the base oil for 1 hour in freeze -19. The unreacted side products will come. Filter the solution and put the base in AC and with HCL37% add pH to 5.5.
Don’t use a flame for heating. Use a bath instead. This setup will give you good results.
)
After adding water. Separate layers. Take the “oil” layer and distill the EA off. Fatter this step. Cool down the base oil for 1 hour in freeze -19. The unreacted side products will come. Filter the solution and put the base in AC and with HCL37% add pH to 5.5.
Don’t use a flame for heating. Use a bath instead. This setup will give you good results.
)
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This was discussed in the main chat few days ago. The general recommendation was to distill the EA off at 55 °C in vacuum (/negative pressure) for improved yield. Is this what you meant, or did you mean to distill at normal pressure at 77 °C (boiling temp of EA)?
This is the first time I read about this and I shall try this.
I will start a thread about maximizing 4-MMC yield and invite you to share your knowledge. You seem to know a lot about this.
This is the first time I read about this and I shall try this.
I will start a thread about maximizing 4-MMC yield and invite you to share your knowledge. You seem to know a lot about this.
Is it possible to bubbling hydrogen chloride gas instead of adding hydrochloric acid during the crystallization stage?
Yes this is a good alternative to using hydrochloric acid, as long as you meant to say "acidification" instead of "crystallization". No acid is added during the crystallization stage.
can we replace NMP also with ethyl acetate and if yes how much for 100gr of 2b4m
- By HIGGS BOSSON
Yes, you can use NMP, DCM, ethyl acetate
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Hey, thanks for sexy video.
I wonder if you know Perrine paper about bupropion synthesis in NMP (Im sure you do, apparently he got an idea to use NMP).
If not, here you go:
Perrine, D. M.; Ross, J. T.; Nervi, S. J.; Zimmerman, R. H. A Short, One-Pot Synthesis of Bupropion (Zyban®, Wellbutrin®). J. Chem. Educ. 2000, 77 (11), 1479– 1480, DOI: 10.1021/ed077p1479
If you carefully read SI you will see that they had to wash out methylamine from organic layer. Had to be couple of times of water washing. In your procedure you don't even wash organic (benzene) layer, thus I wonder if you ever check melting point? Seems it might be mix of 4mmc and methylamine hydrochloride.
I wonder if you know Perrine paper about bupropion synthesis in NMP (Im sure you do, apparently he got an idea to use NMP).
If not, here you go:
Perrine, D. M.; Ross, J. T.; Nervi, S. J.; Zimmerman, R. H. A Short, One-Pot Synthesis of Bupropion (Zyban®, Wellbutrin®). J. Chem. Educ. 2000, 77 (11), 1479– 1480, DOI: 10.1021/ed077p1479
If you carefully read SI you will see that they had to wash out methylamine from organic layer. Had to be couple of times of water washing. In your procedure you don't even wash organic (benzene) layer, thus I wonder if you ever check melting point? Seems it might be mix of 4mmc and methylamine hydrochloride.