HRID2235236

反应详情

EQUATION

反应方程式

HRID 2235236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Dissolve (4-benzyloxy-2,6-dichloro-phenyl)-methanol in 2.5 L THF and cool to 0° C. under N2. Add 94.45 g PBr3 dropwise and stir at 0° C. for 30 minutes. Pour the reaction mixture into sat'd. NaHCO3 and extract with EtOAc (2×). Dry over Na2SO4, filter and concentrate under vacuum to yield 269 g (89%) of the title compound as a white solid. MS (electrospray), 345.1, 347.1 (ES−).

WORKUP

后处理

  1. additionPour the reaction mixture into sat'd
  2. extractionNaHCO3 and extract with EtOAc (2×)
  3. dry with materialDry over Na2SO4
  4. filtrationfilter
  5. concentrationconcentrate under vacuum