HRID649168

反应详情

EQUATION

反应方程式

HRID 649168 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a stirred solution of 21 g of 3-methoxythiophene in diethyl ether at -40° C. was added 115 ml of a 1.6 molar hexane solution of n-butyllithium. The mixture was warmed slowly over 10 minutes to 0° C., then refluxed for 1 hour, was cooled to -78° C. and a solution containing 21.4 g of dimethyldisulphide in 100 ml of diethyl ether was added. The reaction mixture was warmed to room temperature and stirred for 30 minutes, was poured into water and the organic layer washed with water, with brine, and was then dried over magnesium sulphate and evaporated to dryness.

WORKUP

后处理

  1. temperatureThe mixture was warmed slowly over 10 minutes to 0° C.
  2. temperaturerefluxed for 1 hour
  3. additionwas added
  4. temperatureThe reaction mixture was warmed to room temperature
  5. washthe organic layer washed with water, with brine
  6. dry with materialwas then dried over magnesium sulphate
  7. customevaporated to dryness