تفاعل #1662

معادلة التفاعل

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

H2O

HCl

→

colorless liquid

المردود 79.0%

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

المردود 79.0%

المذيبات

ether

triethylamine

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر