HRID217461

反应详情

EQUATION

反应方程式

HRID 217461 的结构方程式

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of methyl 4-(bromomethyl)-2-{[tert-butyl(dimethyl)silyl]oxy}benzoate (0.30 g) and triethylphosphite (0.17 g) was mixed at 25° C. and then stirred at 130° C. for 24 hours. The reaction liquid was concentrated under reduced pressure and azeotroped with toluene twice (30 mL×2). The residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=40:60 to 10:90) to obtain methyl 2-{[tert-butyl(dimethyl)silyl]oxy}-4-[(diethoxyphosphoryl)methyl]benzoate (0.23 g) as a colorless liquid

WORKUP

后处理

  1. additionwas mixed at 25° C.
  2. customThe reaction liquid
  3. concentrationwas concentrated under reduced pressure
  4. customazeotroped with toluene twice (30 mL×2)
  5. customThe residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=40:60 to 10:90)