Phosphorus oxychloride → 2,4-Dichloro-3,5-dinitrobenzonitrile
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]([NH2:6])=O.P(Cl)(Cl)(Cl)=O>>[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]#[N:6]Komponenten
3
Versuchsvorschrift
A mixture of 66.0 gm. (0.235 mole) of 2,4-dichloro-3,5-dinitrobenzamide and 140 ml. of phosphorus oxychloride is heated at reflux for 1 hour. The solution is cooled to room temperature. The excess phosphorus oxychloride is distilled off in vacuo. The solid residue is triturated with ice-water and filtered. There is obtained 54.0 g. (88%) of a tan solid melting at 139°-141°.
Aufarbeitung
- additionA mixture of 66.0 gm
- temperatureat reflux for 1 hour
- distillationThe excess phosphorus oxychloride is distilled off in vacuo
- customThe solid residue is triturated with ice-water
- filtration