HRID866912

反应详情

EQUATION

反应方程式

HRID 866912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the mixture of 1ml of water and 600mg of potassium hydroxide in 9ml of ethanol was added 200mg of 9-cyano-2-methoxy-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin and the resulting mixture was heated under reflux overnight. Water was added to the mixture, which was washed with benzene. Aqueous layer was acidified with hydrochloric acid, extracted with chloroform, washed with water and dried over anhydrous sodium sulfate. The solvent was evaporated therefrom and there was obtained 130mg of 9-carboxy-2-methoxy-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin having a melting point of 157°-160° C.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux overnight
  3. washwas washed with benzene
  4. extractionextracted with chloroform
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated