Hydrofluoric Acid → 4,4,5,5-Tetrachloro-2,2-difluoro-1,3-dioxolane

温度

200 °C

A 360 mL "Hastelloy" C shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane.

1. customsealed under nitrogen
2. customevacuated
3. customflushed with nitrogen
4. temperatureThe tube was next chilled in an ice-water bath
5. customto remove the excess SF4 and HF
6. waitto stand a day
7. customThe organic phase was separated from the aqueous phase in a polyethylene separatory funnel
8. stirringstirred with a 30% aqueous solution of potassium carbonate
9. dry with materialThe product was dried over potassium carbonate
10. distillationdistilled at a reduced pressure

ORDレコード

ord-c09d5f1396404a9b833dd5912edef351

出典データセット

uspto-grants-1984_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04485250