HRID1986208
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
- 90 °C
PROCEDURE
实验过程
A mixture of 6-bromobenzo[b]thiophene (2.0 g, 9.4 mmol) and sodium thiomethoxide (1.30 g, 18.8 mmol) in DMF (15 mL) is stirred at 90° C. under nitrogen for 6 hours. The reaction is cooled to room temperature, extracted with ethyl acetate and saturated aqueous sodium chloride, washed with 2 N aqueous NaOH solution, saturated aqueous sodium chloride, dried over Na2SO4, filtered, and evaporated. The residue is purified by chromatography on silica gel, eluting with ethyl acetate:hexanes 3:7, to give the title product as a red liquid (1.41 g) which is used for next reaction without further purification.
WORKUP
后处理
- temperatureThe reaction is cooled to room temperature
- extractionextracted with ethyl acetate and saturated aqueous sodium chloride
- washwashed with 2 N aqueous NaOH solution, saturated aqueous sodium chloride
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated
- customThe residue is purified by chromatography on silica gel
- washeluting with ethyl acetate:hexanes 3:7