HRID1009867

反应详情

EQUATION

反应方程式

HRID 1009867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an acetonitrile solution (6 mL) of 2,3,4,6-tetra-O-benzyl-1-C-[2-(benzyloxy)-5-[hydroxy[4-[2-(tritylamino)ethyl]phenyl]methyl]-4-methylphenyl]-D-glucopyranose (0.638 g, 0.565 mmol) were added under nitrogen atmosphere at 0° C. Et3SiH (0.27 mL, 1.695 mmol) and BF3.Et2O (1.58 mL, 1.24 mmol), and the mixture was stirred for 30 minutes at the same temperature. To the reaction solution cooled in ice was added a saturated sodium bicarbonate aqueous solution and the resulting mixture was extracted with ethyl acetate. The organic layer was dried with anhydrous magnesium sulfate. The drying agent was filtered off, and the solvent was evaporated under reduced pressure. Thus obtained residue was purified with silica gel column chromatography (hexane:ethyl acetate=9:1) to obtain the title compound (0.402 g, 59%) as a pale yellow oily compound.

WORKUP

后处理

  1. temperatureTo the reaction solution cooled in ice
  2. extractionthe resulting mixture was extracted with ethyl acetate
  3. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  4. filtrationThe drying agent was filtered off
  5. customthe solvent was evaporated under reduced pressure
  6. customThus obtained residue was purified with silica gel column chromatography (hexane:ethyl acetate=9:1)