反应详情

N-Methylpiperazine (0.620 ml, 5.6 mmol, 2 eq) was added at 0° C. to a solution of benzyl 2,2-dimethyl-4-oxocyclohexylcarbamate (770 mg, 2.8 mmol, 1 eq) in dichloromethane (15 ml), and stirring was carried out for 2 h at RT. Na(OAc)3BH (1.78 g, 8.4 mmol, 3 eq) was added in portions at 0° C., and stirring was carried out for 18 h at RT. The reaction solution was diluted with dichloromethane (60 ml), washed with water (50 ml) and sat. NaCl solution (50 ml), dried over sodium sulfate and concentrated under reduced pressure. After purification by column chromatography (Alox neutral, 1% MeOH in dichloromethane), a white solid was obtained. Yield: 44% (440 mg, 1.225 mmol).

1. stirringstirring
2. waitwas carried out for 18 h at RT
3. washwashed with water (50 ml) and sat. NaCl solution (50 ml)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customAfter purification by column chromatography (Alox neutral, 1% MeOH in dichloromethane)
7. customa white solid was obtained