反应详情

Into 50 ml of dichloroethane was dissolved 1.81 g of 4-[(2S,5R)-4-benzyl-2,5-dimethylpiperazin-1-yl]-2-methylbenzonitrile, and then 1.62 g of 1-chloroethyl chlorocarbonate was added thereto, followed by heating under refluxing overnight. After the reaction solution was concentrated, 50 ml of methanol was added thereto, followed by heating under refluxing overnight. After the reaction solution was concentrated, water was added thereto, followed by washing with ether. The aqueous phase was made basic with a 1M sodium hydroxide aqueous solution, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then solvent was removed by evaporation to obtain 1.11 g of the title compound.

1. temperatureby heating
2. temperatureunder refluxing overnight
3. concentrationAfter the reaction solution was concentrated
4. addition50 ml of methanol was added
5. temperatureby heating
6. temperatureunder refluxing overnight
7. concentrationAfter the reaction solution was concentrated
8. additionwater was added
9. washby washing with ether
10. extractionfollowed by extraction with ethyl acetate
11. dry with materialThe organic layer was dried over anhydrous sodium sulfate
12. customsolvent was removed by evaporation