反应详情

LiAlH4 (2.10 g, 55 mmol) and THF (150 ml) were placed in a dry ballon. After cooling this mixture to 0° C. a solution of (trans-4-acetylamino-cyclohexyl)-acetic acid ethyl ester (8.42 g, 37 mmol) in little THF was added dropwise. The reaction was stirred 1 h before careful neutralization with H2O (5.6 ml), 1 N NaOH (3×5.6 ml) and more H2O (5.6 ml). The resulting mixture was stirred over night before filtering off the solids. Evaporation of the solvent and drying under high vacuum afforded 5.25 g (76%, 28 mmol) of a light brown solid. MS (m/z): 186.4 ([M+H+).

1. additionwas added dropwise
2. filtrationbefore filtering off the solids
3. customEvaporation of the solvent
4. customdrying under high vacuum