HRID1164953

反应详情

EQUATION

反应方程式

HRID 1164953 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 7.0 g (45 mmol) of 4-nitrothiophenol and 22.5 mL of 4N aqueous potassium hydroxide in 40 mL of dimethylformamide add a solution of 9.53 g (55 mmol) of 2-chloro-N,N-diethylethanamine hydrochloride in 40 mL of dimethylformamide. Heat the reaction mixture for about 3 h at 100° C. After this time, cool the mixture to room temperature and add 150 mL of water. Extract th aqueous mixture with 3×200 mL of methylene chloride. Combine the methylene chloride extracts and extract these with 200 mL of 1N aqueous hydrochloric acid. Make the acid extract basic with saturated aqueous sodium bicarbonate solution

WORKUP

后处理

  1. temperatureAfter this time, cool the mixture to room temperature
  2. extractionExtract th aqueous mixture with 3×200 mL of methylene chloride
  3. extractionextract these with 200 mL of 1N aqueous hydrochloric acid
  4. extractionextract basic with saturated aqueous sodium bicarbonate solution