HRID1009865

反应详情

EQUATION

反应方程式

HRID 1009865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To an acetonitrile solution (8.8 mL) of (1S)-1,5-anhydro-2,3,4,6-tetra-O-benzyl-1-[2-(benzyloxy)-5-(4-bromobenzyl)-4-methylphenyl]-D-glucitol (780 mg, 0.876 mmol) were added vinyl acetate (184 mg, 2.14 mmol), palladium(II) acetate (20 mg, 0.0890 mmol), tri-O-tolylphosphine (54 mg, 0.177 mmol) and triethylamine (0.64 mL, 4.38 mmol), and reacted at 120° C. for 20 minutes with microwave manufactured by Biotage. The reaction solution was evaporated under reduced pressure. Thus obtained residue was purified with silica gel column chromatography (hexane:ethyl acetate=5:1, chloroform:methanol=40:1) to obtain the title compound (681 mg, 87%) as an orange-yellow amorphous compound.

WORKUP

后处理

  1. customreacted at 120° C. for 20 minutes with microwave
  2. customThe reaction solution was evaporated under reduced pressure
  3. customThus obtained residue was purified with silica gel column chromatography (hexane:ethyl acetate=5:1, chloroform:methanol=40:1)