HRID455252

反应详情

EQUATION

反应方程式

HRID 455252 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NaBH4 (200 mg, 5.3 mmol) was added to a solution of (2S,4R)-4-(tert-Butyl-diphenyl-silanyloxy)-1-(4-trifluoromethoxy-phenylcarbamoyl)-pyrrolidine-2-carboxylic acid methyl ester (2.8 g, 4.8 mmol) in methanol (50 mL) portion-wise. The mixture was stirred at room temperature for 4 hours. Then the mixture was poured into water (50 mL), extracted with ethyl acetate (3×50 mL). The organic layers was combined, washed with brine (50 mL), dried over anhydrous sodium sulphate, filtered and concentrated. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate=5:1) to give 2.35 g (88%) of the title compound.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×50 mL)
  2. washwashed with brine (50 mL)
  3. dry with materialdried over anhydrous sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate=5:1)