HRID750318

反应详情

EQUATION

反应方程式

HRID 750318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-acetyl-2-(4-acetylbenzyl)-6-bromo-4-phenyl-2H-isoquinolin-1-one (95 mg) in ethanol (10 ml) were added hydroxylamine hydrochloride (17 mg) and sodium acetate (29 mg) at room temperature and the mixture was heated under reflux for 6 hrs. The solvent was evaporated under reduced pressure and the residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate solution, washed with saturated brine and dried by adding sodium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1→3/2) to give the title compound (84 mg, 86%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 6 hrs
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate solution
  5. washwashed with saturated brine
  6. customdried
  7. additionby adding sodium sulfate
  8. customThe solvent was evaporated under reduced pressure
  9. customthe obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1→3/2)