HRID1986208

反应详情

EQUATION

反应方程式

HRID 1986208 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction is cooled to room temperature
  2. extractionextracted with ethyl acetate and saturated aqueous sodium chloride
  3. washwashed with 2 N aqueous NaOH solution, saturated aqueous sodium chloride
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is purified by chromatography on silica gel
  8. washeluting with ethyl acetate:hexanes 3:7