HRID1672633
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
A solution of 5.95 g (22.86 mmol) of {5-fluoro-2-[2-(4-methoxyphenyl)ethyl]phenyl}methanol from Example 31A in 130 ml of acetonitrile is mixed with 7.45 g (21.71 mmol) of triphenylphosphonium hydrobromide and heated to reflux for 3 hours. The reaction solution is then concentrated to dryness, and the resulting oil is taken up and triturated in diethyl ether. The product crystallizes as a white solid during this. After filtration, the solid is dried in a drying oven at 50° C. overnight. 11.5 g (77% yield) of crystalline product are obtained.
WORKUP
后处理
- temperatureheated
- temperatureto reflux for 3 hours
- concentrationThe reaction solution is then concentrated to dryness
- customtriturated in diethyl ether
- customThe product crystallizes as a white solid during this
- filtrationAfter filtration
- customthe solid is dried in a drying oven at 50° C. overnight