HRID1856815
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 suspension of 4.0 g (8.1 mmol) of (2-hydroxy-5-nitrophenyl) methyltriphenylphosphonium bromide in 50 ml of toluene is heated to reflux, then 5.1 ml (36 mmol) of triethylamine and 1.9 g (12 mmol) of 4,4,4-trifluorobutyryl chloride are added. The mixture is stirred for 2 hours, then it is filtered and the filtrate is concentrated under reduced pressure. By chromatography of the residue on a silica column using a 0-30% mixture of dichloromethane in cyclohexane, 1.1 g of product are obtained. Melting point: 70-71° C.
WORKUP
后处理
- temperatureis heated
- temperatureto reflux
- filtrationit is filtered
- concentrationthe filtrate is concentrated under reduced pressure
- customare obtained