HRID13757

反应详情

EQUATION

反应方程式

HRID 13757 的结构方程式

PROCEDURE

实验过程

6.20 g of ethyl 4-(bromomethyl)-3-trifluoromethylbenzoate (Reference Example 2 (step 2)) was dissolved in 12 ml of trimethyl phosphite and the mixture was heated at reflux for 4 hours under an argon atmosphere. After the completion of the reaction, the operation of adding of toluene to the residue, followed by azeotropic removal of trimethyl phosphite was repeated three times. The residue was purified by silica gel column chromatography to obtain 4.96 g of the objective compound as a yellow oily product.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 4 hours under an argon atmosphere
  3. customAfter the completion of the reaction
  4. customfollowed by azeotropic removal of trimethyl phosphite
  5. customThe residue was purified by silica gel column chromatography