반응 #1073588

반응 방정식

HCl

n-Butyllithium

4-ethoxyphenyl acetonitrile

dichloroethane

→

1-cyano-1-(4-ethoxyphenyl)cyclopropane

용매

THF

THF

반응 조건

후처리

1. 1
   농축concentrated under reduced pressure
2. 2
   추출extracted with diethyl ether (x3)
3. 3
   세척washed with water
4. 4
   건조dried over anhydrous sodium sulphate
5. 5
   기타the solvent removed under reduced pressure
6. 6
   workup.DISTILLATIONthe residue distilled
7. 7
   기타to give the product, b.p. 116°-120° C., yield 40 g

실험 절차

1.6M n-Butyllithium (680 ml) is added over 5 min to a stirred solution of 4-ethoxyphenyl acetonitrile (56 g) in anhydrous THF (600 ml) at 25° C. under an atmosphere of nitrogen. After 1 h, a solution of 1.2 dichloroethane (111 g) in anhydrous THF (300 ml) is added dropwise over 2 h and the mixture stirred at 25° C. for 16 h. The mixture is then poured onto 3N HCl (1 l ), concentrated under reduced pressure, extracted with diethyl ether (x3), washed with water, dried over anhydrous sodium sulphate, the solvent removed under reduced pressure and the residue distilled to give the product, b.p. 116°-120° C., yield 40 g. nD 1.5320.

출처