Реакция #1662

Уравнение реакции

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

H2O

HCl

→

colorless liquid

Выход 79.0%

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

Выход 79.0%

Растворители

ether

triethylamine

Условия реакции

Обработка

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

Методика

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.

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