反応 #58965

反応方程式

1-(2-bromoethyl)-4-nitrobenzene

pyrazole

potassium hydroxide

→

1-[2-(4-nitrophenyl)ethyl]-1H-pyrazole

収率 8.0%

溶媒

water

反応条件

後処理

1. 1
   抽出the mixture was extracted with ethyl acetate
2. 2
   洗浄The organic layer was washed with water
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   濃縮concentrated

実験手順

A mixture of 1-(2-bromoethyl)-4-nitrobenzene (18.7 g), pyrazole (5.53 g) and potassium hydroxide (4.56 g) was stirred at 140° C. for 8 min. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to give 1-[2-(4-nitrophenyl)ethyl]-1H-pyrazole (1.37 g, 8%) as crystals from a fraction eluted with hexane-ethyl acetate (1:2, v/v). Recrystallization thereof from ethyl acetate-hexane gave yellow prism crystals. melting point: 92-93° C.

出典