HRID1856815

反应详情

EQUATION

反应方程式

HRID 1856815 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureis heated
  2. temperatureto reflux
  3. filtrationit is filtered
  4. concentrationthe filtrate is concentrated under reduced pressure
  5. customare obtained