HRID235597

反应详情

EQUATION

反应方程式

HRID 235597 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of quinoline-6-carboxaldehyde (5.29 g) and 1-triphenylphosphoranylidene-2-propanone (1.5 equiv) in dimethyl sulfoxide (100 ml) was stirred at room temperature for 24 hr. The solution was poured into water (600 ml) which was subsequently extracted with ethyl acetate. The dried (MgSO4) organic fraction was evaporated under reduced pressure and the residue was purified by column chromatography over silica with dichloromethane/ethyl acetate (4:1 v/v) elution to give 1-(quinolin-6-yl)but-1-ene-3-one as a white solid. Pmr spectrum (CDCl3 ; δ in ppm : 2.41 (3H,s); 6.83 (1H,d); 7.3-9.0 (7H,m).

WORKUP

后处理

  1. extractionwas subsequently extracted with ethyl acetate
  2. dry with materialThe dried (MgSO4) organic fraction
  3. customwas evaporated under reduced pressure
  4. customthe residue was purified by column chromatography over silica with dichloromethane/ethyl acetate (4:1 v/v) elution