Réaction #1595

Équation de réaction

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

H2O

HCl

→

colorless liquid

Rendement 79.0%

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

Rendement 79.0%

Solvants

ether

triethylamine

Conditions de réaction

Traitement

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

Mode opératoire

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 atmospheric pressure from 64°-68° C. to yield 36 g (79%) of a colorless liquid as pure product.

Source