HRID397719

反应详情

EQUATION

反应方程式

HRID 397719 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 2-(4,4-dimethylcyclohexyl)acetate (Preparation 14, 2.0 g, 10 mmol) in tetrahydrofuran (20 ml) under an atmosphere of nitrogen at 0° C. was added lithium aluminium hydride (1.0M solution in tetrahydrofuran, 11 ml, 11 mmol) and the reaction mixture was allowed to warm to room temperature overnight. The mixture was poured onto ice (300 g), acidified to pH 1 with 1N aqueous hydrochloric acid and extracted with dichloromethane (200 ml). The organic extract was dried (MgSO4), filtered and concentrated in vacuo to afford the title compound as a pale yellow oil (1.45 g, 93%).

WORKUP

后处理

  1. additionThe mixture was poured onto ice (300 g)
  2. extractionextracted with dichloromethane (200 ml)
  3. extractionThe organic extract
  4. dry with materialwas dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo