HRID37244

反应详情

EQUATION

反应方程式

HRID 37244 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 0.110 g (0.31 mmol) of the product of Step A dissolved in 1.0 mL of carbon tetrachloride was added 0.03 mL (1.6 mmol) of phosphorous tribromide and the reaction mixture was stirred at room temperature for 10 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 15% EtOAc-hexane. The purified fractions were evaporated in vacuo affording 0.104 g (80%) 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 15% EtOAc-hexane
  5. customThe purified fractions were evaporated in vacuo