HRID1171714

反应详情

EQUATION

反应方程式

HRID 1171714 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium borohydride (300 mg) was added to a solution of (E)-3-{[1-(t-butoxycarbonyl)-5-(ethoxycarbonylmethyl)-1H-pyrazol-3-yl]methylidene}-1-(triphenylmethyl)piperidin-4-one (9.64 g) in ethanol (100 ml) at 0° C. After the mixture was stirred at the same temperature for 1.5 hours, the reaction was quenched by addition of a saturated aqueous ammonium chloride solution. The product was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. Evaporation of the solvent under reduced pressure followed by purification of the residue by silica gel chromatography using hexane, ethyl acetate, and dichloromethane (1:1:1) as eluent gave the title compound (7.7 g, yield: 80%) as a pale yellow amorphous solid.

WORKUP

后处理

  1. customthe reaction was quenched by addition of a saturated aqueous ammonium chloride solution
  2. extractionThe product was extracted with ethyl acetate
  3. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customEvaporation of the solvent under reduced pressure
  6. customfollowed by purification of the residue by silica gel chromatography