HRID2192886
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of 2-bromobenzenethiol (50 g) in DMF (500 mL) were added bromocyclopropane (41.6 g), potassium carbonate (54.8 g), and triphenylmethanethiol (1.46 g), followed by stirring at an internal temperature of 80° C. for 24 hours. After cooling to room temperature, water and ethyl acetate were added thereto, and the organic layer was then separated. The organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 1-bromo-2-(cyclopropylsulfanyl)benzene (49.3 g).
WORKUP
后处理
- temperatureAfter cooling to room temperature
- customthe organic layer was then separated
- washThe organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography