HRID216338

反应详情

EQUATION

反应方程式

HRID 216338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To 2,2-difluoro-1-(2-fluoro-4-methoxyphenyl)ethanone (45.0 g, 0.22 mol) in 400 mL of CH2Cl2 at −78° C. was added BBr3 (165.67 g, 0.66 mol) in 100 mL of CH2Cl2 dropwise. The resulting solution was stirred overnight at 25° C., and was quenched by dropwise addition of CH3OH (900 mL) at −30° C. and after stirring for 2 hours at −30° C. and for 1 hour at 25° C., the solvents were evaporated and the residue was purified by column chromatography (PE/EA 6:1) to afford 2,2-difluoro-1-(2-fluoro-4-hydroxyphenyl)ethanone as a solid.

WORKUP

后处理

  1. customwas quenched by dropwise addition of CH3OH (900 mL) at −30° C.
  2. stirringafter stirring for 2 hours at −30° C. and for 1 hour at 25° C.
  3. customthe solvents were evaporated
  4. customthe residue was purified by column chromatography (PE/EA 6:1)