Reaktionsgleichung
[CH:1](Cl)([O:6][CH:7]([F:9])[F:8])[C:2]([F:5])([F:4])[F:3].[F-:11].[K+]>>[CH:7]([O:6][CH:1]([C:2]([F:5])([F:4])[F:3])[F:11])([F:9])[F:8]Komponenten
Reaktionsbedingungen
- Temperatur
- 278 °C
Versuchsvorschrift
A 1 liter autoclave (316SS, Parr) was charged with 171 g (0.93 moles) isoflurane and 116 g (2.0 moles) potassium fluoride. The reaction mass was heated with stirring to 278° C. After 18 hours at 278° C., the pressure was 500 psi. The autoclave was then cooled to room temperature for transfer to the laboratory. Products were then distilled into a dry ice cooled trap by heating the autoclave on a hot plate. The trap contents (134 g) were distilled through a four foot vacuum jacketed column packed with glass beads to give 20.8 g CHF2OCHFCF3 (bp 23.5° C.). The material remaining in the distillation flask (104.0 g) was 98% isoflurane. Based on the materials isolated, the percent conversion was 13% (33% yield). Details of the distillation are given below.
Aufarbeitung
- temperatureThe reaction mass was heated
- temperatureThe autoclave was then cooled to room temperature for transfer to the laboratory
- distillationProducts were then distilled into a dry ice cooled trap
- temperatureby heating the autoclave on a hot plate
- distillationThe trap contents (134 g) were distilled through a four foot vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-90d092d4aa6546c4878274d19f605a91
- Quelldatensatz
- uspto-grants-1989_10
- Patentnummer
- US04874901
Verknüpfte Notizen
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