反应详情

A 0.92 ml portion of 1-chloroethyl chloroformate was added to 20 ml of dichloroethane solution containing 0.31 g of (2S,5R)-4-(4-benzyl-2,5-dimethylpiperazin-1-yl)-2-trifluoromethylbenzonitrile, and the mixture was stirred for 2 days with heating under reflux. The reaction mixture was concentrated, mixed with 20 ml of methanol and then stirred for 1 day with heating under reflux. The reaction mixture was concentrated and the residue was subjected to a silica gel column chromatography and purified with chloroform-methanol (9:1, v/v) to obtain 0.19 g of the title compound as a yellow oil.

1. temperaturewith heating
2. temperatureunder reflux
3. concentrationThe reaction mixture was concentrated
4. additionmixed with 20 ml of methanol
5. stirringstirred for 1 day
6. temperaturewith heating
7. temperatureunder reflux
8. concentrationThe reaction mixture was concentrated
9. custompurified with chloroform-methanol (9:1