反应详情

温度

10 °C

To a solution of 4-(4-cyclopropyl-piperazine-1-carbonyl)-benzaldehyde (56.0 g) in 1,2-dichloroethane (550 mL) was added morpholine (37.8 mL) dropwise over 5 min. The mixture was cooled to 10° C. and was treated with NaBH(OAc)3 (64.3 g) in portions over 1 h. After a further 2 h, the mixture was warmed to room temperature, and a water bath was used to keep the temperature below 20° C. After 18 h, water (60 mL) was added while the temperature was kept under 20° C. by the addition of small amounts of ice. After 20 min, the mixture was basified to pH ˜10 with 1 N NaOH (450 mL) and the mixture was stirred for 10 min. The layers were separated, and the organic layer was washed with 1 N NaOH (150 mL). The combined aqueous layers were extracted with CH2Cl2 (200 mL). The combined organic layers were washed with brine (200 mL), dried (Na2SO4), and concentrated to yield the title compound as pale yellow viscous oil.

1. temperaturethe mixture was warmed to room temperature
2. customa water bath was used
3. customthe temperature below 20° C
4. waitAfter 18 h
5. additionwas kept under 20° C. by the addition of small amounts of ice
6. waitAfter 20 min
7. customThe layers were separated
8. washthe organic layer was washed with 1 N NaOH (150 mL)
9. extractionThe combined aqueous layers were extracted with CH2Cl2 (200 mL)
10. washThe combined organic layers were washed with brine (200 mL)
11. dry with materialdried (Na2SO4)
12. concentrationconcentrated