HRID750282

反应详情

EQUATION

反应方程式

HRID 750282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was evaporated under reduced pressure
  2. additionthe residue was diluted with ethyl acetate
  3. washwashed with 1N hydrochloric acid
  4. customdried
  5. customThe solvent was evaporated under reduced pressure
  6. addition4N Hydrochloric acid ethyl acetate solution (10 ml) was added to the residue
  7. stirringthe mixture was stirred at room temperature for 18 hrs
  8. filtrationThe precipitate was collected by filtration
  9. washwashed with diethyl ether
  10. customdried