HRID750282
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
- 50 °C
PROCEDURE
实验过程
To a solution of 6-bromo-4-phenyl-3-isocoumarincarboxylic acid (1.25 g) in methanol (20 ml) were added 4-methanesulfonylbenzylamine hydrochloride (1.6 g) and triethylamine (2.5 ml), and the mixture was stirred at 50° C. for 18 hrs. The solvent was evaporated under reduced pressure, and the residue was diluted with ethyl acetate, washed with 1N hydrochloric acid, and dried. The solvent was evaporated under reduced pressure. 4N Hydrochloric acid ethyl acetate solution (10 ml) was added to the residue, and the mixture was stirred at room temperature for 18 hrs. The precipitate was collected by filtration, washed with diethyl ether and dried to give the title compound (1.43 g).
WORKUP
后处理
- customThe solvent was evaporated under reduced pressure
- additionthe residue was diluted with ethyl acetate
- washwashed with 1N hydrochloric acid
- customdried
- customThe solvent was evaporated under reduced pressure
- addition4N Hydrochloric acid ethyl acetate solution (10 ml) was added to the residue
- stirringthe mixture was stirred at room temperature for 18 hrs
- filtrationThe precipitate was collected by filtration
- washwashed with diethyl ether
- customdried