HRID656057
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 ethyl 5-bromo-3-(tetrahydro-3-thienylmethyl)-1H-indole-7-carboxylate (7.61 g, 20.73 mmol) in dichloromethane (150 mL) was added portionwise 3-chlorobenzoperoxoic acid (10.69 g, 62.19 mmol) at room temperature. The resulting solution was stirred for 5 h. Sodium sulfite was added, and the mixture was washed with water, extracted with DCM (3×100 mL), dried (Na2SO4) and concentrated under reduced pressure. The crude product was purified by column on sillal gel (petroleum:ethyl acetate=10:1 to 5:1 to 2:1), giving 3.52 g (42.56%) of the title compound.
WORKUP
后处理
- washthe mixture was washed with water
- extractionextracted with DCM (3×100 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated under reduced pressure
- customThe crude product was purified by column on sillal gel (petroleum:ethyl acetate=10:1 to 5:1 to 2:1)