HRID1595089
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added dropwise at 0° C
- extractionThe reaction mixture was extracted with 200 ml of MTBE
- washthe extract washed with with 3×100 ml of brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- distillationThe residue was distilled at 82-86° C./0.1 Torr