HRID726700
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
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
4,4-Difluoro-1-tosyl-2,3,4,5-tetrahydro-1H-1-benzazepin-5-one (3.00 g) was dissolved in 14 ml of acetic acid, 7 ml of concentrated sulfuric acid was added to the solution and then the resulting mixture was heated at 60° C. for 10 hours. The reaction solution was ice-cooled, adjusted to a basic range with potassium hydroxide and extracted three times with ethyl acetate, and the resulting organic layer was dried over anhydrous potassium carbonate. By evaporating the reaction solvent, 4,4-difluoro-2,3,4,5-tetrahydro-1H-1-benzazepin-5-one was obtained. This product was used in the following reaction without purification.
WORKUP
后处理
- temperaturecooled
- extractionextracted three times with ethyl acetate
- dry with materialthe resulting organic layer was dried over anhydrous potassium carbonate
- customBy evaporating the reaction solvent