HRID1245160

反应详情

EQUATION

反应方程式

HRID 1245160 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-benzyloxybenzoic acid (1.22 g, 2.6548 mmol) was dissolved in methanol (100 ml), trimethylsilyl diazomethane (36.3 g, 10% solution in hexane, 31.8421 mmol) was added thereto under cooling with ice and the mixture was stirred at room temperature for 2 hours. To the reaction solution was added acetic acid (0.5 ml) and the mixture was allowed to stand at room temperature for 16 hours so as to decompose an excessive reagent. The residue obtained by concentration of the reaction solution was purified by silica gel column chromatography (hexane:ethyl acetate=4:1) to give the title compound (1.18 g, 2.5321 mmol, 95%).

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. waitto stand at room temperature for 16 hours
  3. customThe residue obtained by concentration of the reaction solution
  4. customwas purified by silica gel column chromatography (hexane:ethyl acetate=4:1)