反応 #630705

反応方程式

sodium bisulfite

potassium fluoride

fluorosulfonyl difluoroacetyl fluoride

bromine

tetrafluoroethylene

→

FSO2CF2CF2OCF2CF2Br

溶媒

1,1,2-trichloro-1,2,2-trifluoroethane

acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   workup.DISTILLATIONthe mixture was distilled
3. 3
   その他to give a distillate
4. 4
   その他boiling up to 100° C.
5. 5
   その他The organic layer was separated
6. 6
   workup.DISTILLATIONdistilled

実験手順

A mixture of 5.8 g potassium fluoride, 60 ml acetonitrile and 12 ml fluorosulfonyl difluoroacetyl fluoride was heated at 80° C. for one hour. The resulting mixture was placed in a stainless steel autoclave and heated at 50° C. for one hour and 80° C. for one hour with 16 g of bromine and 30 g of tetrafluoroethylene. The reaction mixture was poured into a solution of sodium bisulfite, 50 ml 1,1,2-trichloro-1,2,2-trifluoroethane was added and the mixture was distilled to give a distillate boiling up to 100° C. which contained two layers. The organic layer was separated and distilled to give FSO2CF2CF2OCF2CF2Br, b.p. 106°, confirmed by infrared, nuclear magnetic resonance and mass spectroscopy.

出典