反应详情

温度

60 °C

To methanol (1 kg) were added trans-4-aminocyclohexanol (200 g), benzaldehyde (553 g) and 10% palladium carbon (20 g), and the mixture was stirred under a hydrogen atmosphere at 60° C. for 24 hr. After cooling to room temperature, the catalyst was filtered off and washed with methanol (400 g). The filtrate and washings were added dropwise to water (2 kg) at 50° C. After cooling to room temperature, the precipitate was collected by filtration, washed with water:methanol=2:1 (volume ratio, 400 g) and dried under reduced pressure to give the title compound (472 g, yield 92%) as a white solid.

1. temperatureAfter cooling to room temperature
2. filtrationthe catalyst was filtered off
3. washwashed with methanol (400 g)
4. additionThe filtrate and washings were added dropwise to water (2 kg) at 50° C
5. temperatureAfter cooling to room temperature
6. filtrationthe precipitate was collected by filtration
7. washwashed with water
8. dry with materialmethanol=2:1 (volume ratio, 400 g) and dried under reduced pressure