HRID1874313

反应详情

EQUATION

反应方程式

HRID 1874313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

p-Benzyloxyphenyl acetonitrile (50 g) was added to dry tetrahydrofuran (250 ml) and cooled to −78° C. Lithium HMDS (20.8 g) in tetrahydrofuran (60 ml) was added slowly to the reaction mixture at −70° C. followed by dropwise addition of cyclohexanone (26.6 g. 0.27 mol) and maintaining the temperature at −60° C. for 2 h. The reaction temperature was allowed to rise to 0° C., charged with water (300 ml) and the organic layer was separated. The aqueous layer was then extracted with ethylacetate. The two organic layers were combined, washed with DM water and dried using Na2SO4. The solvent was evaporated under reduced pressure to give 50 g (70.0%) of 1-[cyano(p-benzyloxyphenyl)methyl]-cyclohexanol.

WORKUP

后处理

  1. temperaturemaintaining the temperature at −60° C. for 2 h
  2. customto rise to 0° C.
  3. customthe organic layer was separated
  4. extractionThe aqueous layer was then extracted with ethylacetate
  5. washwashed with DM water
  6. customdried
  7. customThe solvent was evaporated under reduced pressure