HRID1348794

反应详情

EQUATION

反应方程式

HRID 1348794 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 2-[2-(2-chlorophenyl)ethyl]-6-(4-fluoro-3-methylphenyl)-4-methoxycarbonyl-2H-pyridazin-3-one (480 mg, 1.20 mmol) in THF/methanol (2 mL/1 mL), cerium(III) chloride hexahydrate (425 mg, 1.20 mmol) was added at −15° C., followed by the addition of sodium borohydride (45 mg, 1.20 mmol). After stirred for 10 minutes, a saturated aqueous solution of ammonium chloride was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and was concentrated under reduced pressure. Further, the concentrate was purified by column chromatography on silica gel [hexane/ethyl acetate (2/1)] to yield the title compound as a pale yellow syrupy substance (yield: 11.0%).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. concentrationwas concentrated under reduced pressure
  4. customFurther, the concentrate was purified by column chromatography on silica gel [hexane/ethyl acetate (2/1)]