反応 #1960484

反応方程式

2,3-difluorophenol

propargyl bromide

potassium carbonate

→

1,2-difluoro-3-prop-2-ynyloxybenzene

溶媒

ethyl methyl ketone

反応条件

後処理

1. 1
   ろ過The batch is filtered
2. 2
   洗浄the filter residue is washed with MTBE
3. 3
   その他The filtrate is evaporated to dryness
4. 4
   その他the residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1)

実験手順

115.0 g (0.88 mol) of 2,3-difluorophenol are refluxed for 3 h in 1.6 l of ethyl methyl ketone together with 118.2 ml (17.7 mol) of propargyl bromide (80% soln. in toluene) and 146.6 g (138.2 mol) of potassium carbonate. The batch is filtered, and the filter residue is washed with MTBE. The filtrate is evaporated to dryness, and the residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1).

出典