1-Bromo-2-Chloroethane → 1-(2-Chloroethyl)-4-methylpiperazine dihydrochloride

Temperature

50 °C

10 ml of 25% NaOH and 1 ml (9 mmol) of 4-methyl piperazine were added successively into a reaction flask. The mixture was heated up to 50° C., and 1.8 ml (18 mmol) 1-bromo-2-chloroethane was added dropwise. The mixture was reacted at 50° C. for 6 h, then cooled to room temperature. The reaction solution was extracted with ethyl acetate, and the extraction was washed with saturated saline solution and dried over anhydrous sodium sulfate, then filtered. The filtrate was concentrated to dry in a reduced pressure and a small amount of ethanol/NaOH solution was added dropwise into the residue. The mixture was shaken and placed in a refrigerator for standing, then concentrated to dry in a reduced pressure to obtain 0.43 g white solid with the yield of 23%. m.p. 227-230° C.

1. customThe mixture was reacted at 50° C. for 6 h
2. temperaturecooled to room temperature
3. extractionThe reaction solution was extracted with ethyl acetate
4. extractionthe extraction
5. washwas washed with saturated saline solution
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationThe filtrate was concentrated
9. customto dry in a reduced pressure
10. additiona small amount of ethanol/NaOH solution was added dropwise into the residue
11. concentrationconcentrated
12. customto dry in a reduced pressure

ORD record

ord-f63d19f611374c3eaf17a303996a8bfd

Source dataset

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08664238B2