反应详情

Trans-4-aminocyclohexane carboxylic acid hydrochloride (2.00 g, 14.3 mmol) was added in small portions to a stirred, hot (70-85° C.) solution of Red-Al (27.0 g) for 2 h (a semisolid formed), and heating was continued overnight. After 24 h, the reaction mixture was cooled to room temperature and treated with a solution of NaOH (3.8 g) in H2O (34 ml). Following the addition, the reaction was gradually heated to 80° C., and cooled. The toluene layer was separated and the aqueous layer was extracted with CHCl3 (3×100 ml). The organic layers were dried with MgSO4 and then concentrated under reduced pressure to provide the desired compound (1.81 g, 14.0 mmol) as a pure white solid in 50% yield. ES-MS: 130 (M+1).

1. customformed), and
2. temperatureheating
3. waitAfter 24 h
4. additionthe addition
5. temperaturethe reaction was gradually heated to 80° C.
6. temperaturecooled
7. customThe toluene layer was separated
8. extractionthe aqueous layer was extracted with CHCl3 (3×100 ml)
9. dry with materialThe organic layers were dried with MgSO4
10. concentrationconcentrated under reduced pressure