반응 #1662

반응 방정식

1,1,2 trichloro-2,3,3-trifluorocyclobutane

H2O

HCl

→

colorless liquid

수율 79.0%

1,4-dichloro-1,2,2-trifluorocyclobut-3-ene

수율 79.0%

용매

ether

triethylamine

반응 조건

후처리

1. 1
   세척The ether layer was washed with H2O (100 ml), brine (100 ml)
2. 2
   건조dried over anhydrous MgSO4
3. 3
   기타evaporated in vacuo
4. 4
   workup.DISTILLATIONThe residue was distilled fractionally at atmospheric pressure from 64°-68° C.

실험 절차

To a solution of 1,1,2 trichloro-2,3,3-trifluorocyclobutane (55.5 g) in 100 ml of anhydrous ether, triethylamine (40 ml) was added dropwise over 30 min at room temperature, and the mixture was stirred overnight at ambient temperature. The mixture was then stirred with 120 ml H2O and 7.5 ml of concentrated HCl. The ether layer was washed with H2O (100 ml), brine (100 ml), dried over anhydrous MgSO4, and evaporated in vacuo. The residue was distilled fractionally at atmospheric pressure from 64°-68° C. to yield 36 g (79%) of a colorless liquid as pure product.

출처