HRID1520284

反应详情

EQUATION

反应方程式

HRID 1520284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of ethyl (3R)-1-(4-((4,4,4-trifluoro-1-(2-methyl-4-(4,5,6,7-tetrahydro-2H-indazol-2-yl)phenyl)butyl)amino)benzoyl)piperidine-3-carboxylate (9.61 g), THF (32 mL) and ethanol (32 mL) was added 1M aqueous sodium hydroxide solution (32.2 mL), and the mixture was stirred at room temperature for 2 hr. The solvent was evaporated under reduced pressure, the reaction mixture was neutralized with 1M hydrochloric acid (32.2 mL), and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give the title compound as a crudely purified product. The crudely purified product obtained here and separately synthesized crudely purified product (1.68 g) were combined, and recrystallized from a mixed solvent of ethyl acetate-hexane to give the title compound (8.49 g).

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure