HRID1816747

反应详情

EQUATION

反应方程式

HRID 1816747 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

60% Sodium hydride (1.01 g) was added slowly to a suspension of 4,4′-bicyclohexanol (5 g) in N,N-dimethylformamide (50 ml) at ambient temperature, and the mixture was stirred for 6 hours at 80° C. To the mixture was added dropwise n-propylbromide (2.29 ml) at 0-5° C., and the reaction mixture was stirred for 18.5 hours at 80° C. The reaction mixture was poured into water, and extracted with ethyl acetate. The organic layer was washed with brine and dried, and the solvent was evaporated under reduced pressure. The residue was chromatographed on a column of silica gel eluting with dichloromethane/methyl alcohol (50:1) to give 4′-propyl-4-hydroxy-1,1′-bicyclohexane (1.21 g).

WORKUP

后处理

  1. stirringthe reaction mixture was stirred for 18.5 hours at 80° C
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. customdried
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was chromatographed on a column of silica gel eluting with dichloromethane/methyl alcohol (50:1)