Reaktion #1662

Reaktionsgleichung

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

H2O

HCl

→

colorless liquid

Ausbeute 79.0%

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

Ausbeute 79.0%

Lösungsmittel

ether

triethylamine

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle