반응 #95402

반응 방정식

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

용매

ether

반응 조건

후처리

1. 1
   여과the reaction mixture is filtered
2. 2
   세척the filtrate is successively washed with 2 N sodium bicarbonate solution, 2 N hydrochloric acid and water
3. 3
   건조After drying over sodium sulfate
4. 4
   농축the filtrate is concentrated under reduced pressure
5. 5
   기타the resulting oil is purified by column chromatography over silica gel

실험 절차

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.

출처