HRID903632
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To the mixture of 1 ml of water and 600 mg of potassium hydroxide in 9 ml of ethanol was added 200 mg 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 130 mg of 9-carboxy-2-methoxy-10,11-dihydro-11-oxodibenzo[b,f]thiepin having a melting point of 157°-160° C.
WORKUP
后处理
- temperaturethe resulting mixture was heated
- temperatureunder reflux overnight
- washwas washed with benzene
- extractionextracted with chloroform
- washwashed with water
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was evaporated