反应详情

A mixture of (+)-(2S,5R)-1-allyl-2,5-dimethylpiperazine (10.6 g, 68.7 mmol, prepared according to the literature procedure described by Janetka, J. W. et al., J. Org. Chem., 2003, 68, 3976-3980), 1-chloro-3-iodo-propane (16.9 g, 82.8 mmol, 1.2 eq), and K2CO3 (24.6 g, 178 mmol, 2.6 eq) in acetone (230 mL) was heated at 50° C. for 16 hours. The mixture was cooled to room temperature, filtered through Celite, and the filtrate was concentrated in vacuo. Chromatography on silica gel using a gradient of 2M NH3/MeOH in CH2Cl2 (0-2%) gave 14.05 g (89%) of (2S,5R)-1-allyl-4-(3-chloro-propyl)-2,5-dimethyl-piperazine as a light yellow oil.

1. customprepared
2. filtrationfiltered through Celite
3. concentrationthe filtrate was concentrated in vacuo