反応 #2208

反応方程式

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

H2O

HCl

→

colorless liquid

収率 79.0%

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

収率 79.0%

溶媒

ether

triethylamine

反応条件

後処理

1. 1
   洗浄The ether layer was washed with H2O (100 ml), brine (100 ml)
2. 2
   乾燥dried over anhydrous MgSO4
3. 3
   その他evaporated in vacuo
4. 4
   workup.DISTILLATIONThe residue was distilled fractionally atmospheric pressure from 64°-68° C.

実験手順

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.

出典