HRID241376

反应详情

EQUATION

反应方程式

HRID 241376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl 3-[4-[3-[3-isopropyl-6-(trifluoromethyl)benzothiophen-2-yl]propionyl]-2-methylphenyl]propionate [Example 12 (7)] (70 mg, 0.15 mmol) in EtOH (1.5 ml) was added a solution of hydroxylamine hydrochloride (11 mg, 0.15 mmol) and sodium acetate (14.5 mg, 0.176 mmol) in water (1 mL). The mixture was heated under reflux for 1 hour, cooled at room temperature, diluted with water, and extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was recrystallized from ethyl acetate/hexane to give the titled compound as a pale yellow crystal (55 mg, 57%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 1 hour
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed under reduced pressure
  7. customthe residue was recrystallized from ethyl acetate/hexane