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
To a solution of 1-(4-bromophenyl)cyclopropane carboxylic acid (3.0 g, 12.4 mmol) in dry THF (40 mL) under nitrogen atmosphere, was added borane dimethyl sulphide (8.83 mL, 19.8 mmol, 2 M solution in DCM) at 0° C. The reaction mixture was stirred at r.t for 4 h. After the completion of reaction as confirmed by TLC, the reaction mixture was quenched by dropwise addition of methanol until effervescence stopped. Volatiles were evaporated in vacuo and the compound was diluted with ethyl acetate (80 mL). The organic layer was separated; washed with water (3×10 mL), dried over Na2SO4 and concentrated. The crude product obtained was purified by column chromatography (silica gel, 1:4 EtOAc:Pet Ether) to afford title compound (2.7 g, 96%) as a solid.
WORKUP
后处理
- customAfter the completion of reaction
- customthe reaction mixture was quenched by dropwise addition of methanol until effervescence
- customVolatiles were evaporated in vacuo
- additionthe compound was diluted with ethyl acetate (80 mL)
- customThe organic layer was separated
- washwashed with water (3×10 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated
- customThe crude product obtained
- customwas purified by column chromatography (silica gel, 1:4 EtOAc:Pet Ether)