Phosphorus pentachloride → HCID 13172332, Verbindung
Reaktionsgleichung
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[C:8]([N+:15]([O-:17])=[O:16])=[CH:7][C:3]=1[C:4](O)=[O:5].P(Cl)(Cl)(Cl)(Cl)[Cl:19]>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[C:8]([N+:15]([O-:17])=[O:16])=[CH:7][C:3]=1[C:4]([Cl:19])=[O:5]Komponenten
3
Versuchsvorschrift
A mixture of 75.0 g. (0.2669 mole) of 2,4-dichloro-3,5-dinitrobenzoic acid and 55.59 g. (0.2669 mole) of phosphorus pentachloride is heated at reflux for 90 minutes and cooled to room temperature. The phosphorus oxychloride is distilled off in vacuo. The residue is recrystallized from cyclohexane to yield 75.9 gm. (95%) of yellow needles melting at 99°-101°.
Aufarbeitung
- additionA mixture of 75.0 g
- temperatureat reflux for 90 minutes
- distillationThe phosphorus oxychloride is distilled off in vacuo
- customThe residue is recrystallized from cyclohexane
- customto yield 75.9 gm
Quellen und Nachweise
- ORD-Eintrag
- ord-2b2a1d6b3f7f44aa8710dea916f3f4b5
- Quelldatensatz
- uspto-grants-1978_05
- Patentnummer
- US04091011
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