Synthesis of Pentedrone from a-bromovalerophenone

[WillD]

Reaction scheme:

Reagents:
a-bromovalerophenone- 5 kg,
n-methyl-2-pyrrolidone (NMP) - 20 L,
Methylamine 40% aq.soln - 8 L,
Benzene - 15 L,
Acetone - 30 L,
Hydrochloric acid con.aq.soln - 1,5 L.

Synthesis:
1. 5 kg a-bromovalerophenone added to the reactor or have calculated amount of crude after halogenation reactions.
2. 20 liters n-methyl-2-pyrrolidone poured, start stirring and heating to 40 *C.
3. Upon reaching 40 *C within the mixture, pour 8 liters methylamine 40% aq.soln and continue stirring 20 minutes.
4. Next, we pour 20 liters of clean cold water, stirring a few minutes.
5. Pour 15-20 liters benzene or other suitable extractor, stirring a few minutes.
6. Stop stirring, waiting for the separation of the mixture into two layers.
7. The bottom aqueous layer was drained through the bottom valve of the reactor.
8. 20 liters of ice acetone were poured and add hydrochloric acid with stirring to pH - 5.
9. Overload the mixture in the freezer.
10. Filter on the nutshe-filter, dry.

Notes:
NMP can be replaced by DMSO, DMF, Sulfolane.