反応 #95402

反応方程式

2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropanecarboxylic acid chloride

γ-picoline

2-benzyl-(α-vinyl)-benzyl alcohol

→

2,2-Dimethyl-3-(2',2'-dichlorovinyl)-cyclopropanecarboxylic acid 2benzyl-(α-vinyl)-benzyl ester

溶媒

ether

反応条件

後処理

1. 1
   ろ過the reaction mixture is filtered
2. 2
   洗浄the filtrate is successively washed with 2 N sodium bicarbonate solution, 2 N hydrochloric acid and water
3. 3
   乾燥After drying over sodium sulfate
4. 4
   濃縮the filtrate is concentrated under reduced pressure
5. 5
   その他the resulting oil is purified by column chromatography over silica gel

実験手順

91 g (0.04 mole) of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropanecarboxylic acid chloride are added dropwise, whilst stirring, to 4.6 g (0.05 mole) of γ-picoline, 100 ml of absolute ether and 8.5 g (0.38 mole) of 2-benzyl-(α-vinyl)-benzyl alcohol at 0°-5° C. After having been stirred for 12 hours at 25° C., the reaction mixture is filtered and the filtrate is successively washed with 2 N sodium bicarbonate solution, 2 N hydrochloric acid and water. After drying over sodium sulfate, the filtrate is concentrated under reduced pressure and the resulting oil is purified by column chromatography over silica gel, using toluene as the eluant.

出典