HRID1492646

反应详情

EQUATION

反应方程式

HRID 1492646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.560 g (1.62 mmol) of the product of Step B dissolved in 5.0 mL of carbon tetrachloride was added 154 μL (1.62 mmol) of phosphorous tribromide and the reaction mixture was stirred at room temperature for 5 minutes. Carbon tetrachloride was evaporated from the reaction mixture several times to remove the hydrogen bromide, then the residue was purified on a silica gel flash chromatography column eluted with 5% EtOAc-hexane. The purified fractions were evaporated in vacuo affording 0.523 g (81%) of the title compound.

WORKUP

后处理

  1. customCarbon tetrachloride was evaporated from the reaction mixture several times
  2. customto remove the hydrogen bromide
  3. customthe residue was purified on a silica gel flash chromatography column
  4. washeluted with 5% EtOAc-hexane
  5. customThe purified fractions were evaporated in vacuo