HRID579737

反应详情

EQUATION

反应方程式

HRID 579737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2,3-bis(4-methoxyphenyl)thiophene (5.92 g, 20 mmole) in toluene (20 ml)/diethyl ether (120 ml) was treated with 1.6M n-butyl lithium (14 ml, 1.1 equiv.) and heated at reflux for 1.5 hours. The reaction mixture was cooled to 0° and treated with a solution of cyclohexanone (2.3 ml, 1.1 equiv.) in 5 ml of diethyl ether. The mixture was stirred for 1.5 hours at 0° and 1 hour at room temperature, quenched with water, and extracted with ethyl acetate. The organic extracts were washed with brine, dried and concentrated in vacuo. Chromatography on a Waters Prep 500 (hexane/ethyl acetate, 3:1) provided the title compound (5.8 g, 74%) as an oil.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 1.5 hours
  3. temperatureThe reaction mixture was cooled to 0°
  4. customquenched with water
  5. extractionextracted with ethyl acetate
  6. washThe organic extracts were washed with brine
  7. customdried
  8. concentrationconcentrated in vacuo