反应详情

To a solution of 1-benzyl-4-[(5-chloroisoindol-2-yl)sulfonyl]piperazine (222 mg) in 1,2-dichloroethane (20 ml), 1-chloroethyl chloroformate (81 mg) was added under ice cooling. The resulting mixture was stirred for 15 minutes and then heated under reflux for 1 hour. After cooling, anhydrous methanol was added to the residue obtained by distilling off the solvent under reduced pressure. The mixture was heated under reflux for 11 hours. After cooling, the residue obtained by distilling off the solvent under reduced pressure was purified by chromatography on a silica gel column (ethanol:dichloromethane=1:50 to 1:10), whereby the title compound (120 mg, 70%) was obtained.

1. temperatureheated
2. temperatureunder reflux for 1 hour
3. temperatureAfter cooling
4. customobtained
5. distillationby distilling off the solvent under reduced pressure
6. temperatureThe mixture was heated
7. temperatureunder reflux for 11 hours
8. temperatureAfter cooling
9. customthe residue obtained
10. distillationby distilling off the solvent under reduced pressure
11. customwas purified by chromatography on a silica gel column (ethanol:dichloromethane=1:50 to 1:10), whereby the title compound (120 mg, 70%)
12. customwas obtained