Σύνθεση μεφεδρόνης (4-MMC) σε διαλύτη NMP. Μεγάλης κλίμακας.

[dark_side_of_chemistry]

Στη σύνθεση του 2βρωμο 3 χλωροπριοφενόνιο είναι το ίδιο ?

 

[RichKuklinski]

it is same

 

[Serega]

Παίρνω το πιο καθαρό προϊόν σε DCM, αλλά το κυριότερο είναι να μην αφήσω το διάλυμα να βράσει, να διατηρήσω τη θερμοκρασία όχι υψηλότερη από 36C (το 4-mmc αποδεικνύεται άψογα καθαρό και χιονόλευκο). Μια άλλη πολύ καλή επιλογή είναι το διχλωροαιθάνιο. επίσης καλό αποτέλεσμα επιτυγχάνεται όταν χρησιμοποιείται NMP και τολουόλιο μαζί (αναλογία 3:2).

 

[crisu1542]

What about the DMF ? Do I have to keep the temperature to 36 degrees Celsius here too ? As far as I know the boiling point of dmf is over 130 degrees.

 

[wikimiki]

What if I gonna replace NMP with DMF? Somebody tried? What proportion of DMF should be used if in use instead DMF?

Somebody have the stirring timings and than other timings for those synthesis description? It looks very interesting, I will be appreciate.

 

[William D.]

DMF can be used like DMSO, but yield and some other conditions may differ.

 

[lemon]

DMSO+Toluene = Yield

 

[wikimiki]

William thanks a lot but could you tell me how much differ your recipe if I put DCM and what need to be changed if I put as someone said below DMSO and Toulene? I will be appreciate. With highest respect for the recepture you have posted I cannot get how in large scale production the 40-50% of yield can satisfy you?

Best regards

 

[William D.]

For the test, you must mix BK4, dcm and methylamine as usual. You can add the amount of DMSO until the mixture becomes homogeneous. In this form, the reaction will be faster than usual. You control the reaction for the first time in temperature (when the mixture begins to cool, the reaction is finished, even without additional heating). After you add pure cold water and separate the lower layer and rinse again. Further steps are the same as you used (acidification with acetone or into the water layer)

 

[crisu1542]

1. when swapping NMP for DMF, are the temperatures and pH different ? Solvents have different boiling points and I don't know if this is relevant.
2.Finally, what should be the temperature after adding methylamine ? Once it finds 36, once it finds 40.... Need exact information.
3. is it necessary to heat externally or to cool the solution after adding methylamine ?
4. when acidifying use EA or not ? Once I read that no, once that EA instead of acetone.
5. does the free base if it does not exceed 36 degrees Celsius does not require further cleaning ?

Thanks to all experienced in advance .

 

[CezaryNieStary]

40% roztwór wodny aminy metylowej (CAS 74-89-5can you replace it with something?

 

[Amorking]

The fast way 2iodo4methylenopropiophenone+NMP
Temp need be 35-40 in 9min
With 2bromo4methylenopropiophenone+NMP
Temp need be 55-60 in 20min