HRID1492646
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customCarbon tetrachloride was evaporated from the reaction mixture several times
- customto remove the hydrogen bromide
- customthe residue was purified on a silica gel flash chromatography column
- washeluted with 5% EtOAc-hexane
- customThe purified fractions were evaporated in vacuo