HRID583623

反应详情

EQUATION

反应方程式

HRID 583623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 18.0 g (86 mmol) of 2,3-dimethyl-4-(2,2,3-trimethylcyclopent-3-enyl)butanal in 50 ml of ethanol was added dropwise at 0° C. to 45.0 g (0.11 mol) of sodium borohydride suspended in 200 ml of the same solvent. After 18 hours of stirring at room temperature 100 ml of 1.0 N aqueous hydrochloric acid was added dropwise at 0° C. The reaction mixture was extracted with 200 ml of MTBE, the extract washed with with 3×100 ml of brine, dried (MgSO4) and concentrated in vacuo. The residue was distilled at 82-86° C./0.1 Torr to give 14.1 g (78% yield) of 2,3-dimethyl-4-(2,2,3-trimethylcyclopent-3-enyl)butan-1-ol.

WORKUP

后处理

  1. additionwas added dropwise at 0° C
  2. extractionThe reaction mixture was extracted with 200 ml of MTBE
  3. washthe extract washed with with 3×100 ml of brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. distillationThe residue was distilled at 82-86° C./0.1 Torr