HRID1610160

反应详情

EQUATION

反应方程式

HRID 1610160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

8.4 g of 1-bromo-4-fluoro-2-methoxy-benzene obtained in Production Example II-1-a was dissolved in 200 ml of dichloromethane. 21 ml of titanium tetrachloride and 5.6 ml of dichloromethyl methyl ether were added at 0° C. in nitrogen atmosphere, followed by stirring at room temperature for 4.5 hours. Then, the reaction mixture was gradually poured onto ice-water, and extracted with diethyl ether for two times. The organic layer was sequentially washed with each one portion of water, saturated aqueous sodium hydrogencarbonate solution and water, dried over magnesium sulfate and the solvent was evaporated, to give 9.44 g of the title compound as white crystals.

WORKUP

后处理

  1. additionThen, the reaction mixture was gradually poured onto ice-water
  2. extractionextracted with diethyl ether for two times
  3. washThe organic layer was sequentially washed with each one portion of water, saturated aqueous sodium hydrogencarbonate solution and water
  4. dry with materialdried over magnesium sulfate
  5. customthe solvent was evaporated