HRID1055549

反应详情

EQUATION

反应方程式

HRID 1055549 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 (2S,3R,4S,5S,6R)-2-[4-chloro-3-[[4-(2,2,2-trifluoroethoxyl)phenyl]methyl]phenyl]-6-(hydroxymethyl)-2-methoxy-tetrahydropyran-3,4,5-triol 17e (3.5 g, 7.1 mmol) in dichloromethane (60 mL) were added imidazole (0.97 g, 14.2 mmol) and tert-butyldimethylsilyl chloride (2.14 g, 14.2 mmol) in turn at 0° C. The mixture was warmed up to room temperature and stirred for 2 hours. The reaction mixture was adjusted with saturated aqueous sodium bicarbonate to pH 7 and partitioned. The organic layer was washed with saturated aqueous sodium chloride (50 mL), dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo to give the title compound 17f as light yellow oil (4.8 g, 100%). This material was not further purified.

WORKUP

后处理

  1. custompartitioned
  2. washThe organic layer was washed with saturated aqueous sodium chloride (50 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo