Reaktionsgleichung
[CH3:1][C:2]1[C:10]2[O:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)(Cl)Cl.[ClH:17].[Cl:18]Cl>C(Cl)(Cl)(Cl)Cl>[CH3:1][C:2]1[C:10]2[O:9][C:8]([Cl:18])([Cl:17])[O:7][C:6]=2[CH:5]=[CH:4][CH:3]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
160 g of 4-methyl-1,3-benzodioxole are added dropwise to 276 g of phosphorus pentachloride in 840 ml of carbon tetrachloride (prepared from phosphorus trichloride and chlorine), with stirring. Vigorous evolution of hydrogen chloride starts immediately. Towards the end of the reaction, 85 g of chlorine are passed in at about 20° C. and when the evolution of gas has ended, the mixture is then heated under reflux. By distillation, the phosphorus trichloride and carbon tetrachloride are recovered and the 4-methyl-2,2-dichloro-1,3-benzodioxole is then obtained at boiling point: 98-99° C. (22 mbar).
Aufarbeitung
- customare passed in at about 20° C. and when
- temperaturethe mixture is then heated
- temperatureunder reflux
- distillationBy distillation
- customthe phosphorus trichloride and carbon tetrachloride are recovered
Quellen und Nachweise
- ORD-Eintrag
- ord-0ce8641352074532a813a695ba1e500a
- Quelldatensatz
- uspto-grants-1989_12
- Patentnummer
- US04886816
Verknüpfte Notizen
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