Phosphorus oxychloride → HCID 13530389, Verbindung
Reaktionsgleichung
[C:1]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]1[CH:12]=[CH:13][C:14](=O)[NH:15][N:16]=1)(=[O:3])[CH3:2].P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:14]1[N:15]=[N:16][C:11]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][C:1](=[O:3])[CH3:2])=[CH:12][CH:13]=1Komponenten
3
Versuchsvorschrift
A mixture of 6-(2-acetoxyphenyl)-3(2H)pyridazinone (22.4g) and phosphoryl chloride (90 ml) was stirred and warmed at 55°-60° for 40 minutes. The phosphoryl chloride was removed under reduced pressure at 50° and the residual oil was poured on to ice (200 g). The mixture was allowed to stand overnight at 5° and was filtered to give 3-chloro-6-(2-acetoxyphenyl)pyridazine (23.1 g m.p. 131°-133.5°. A sample recrystallised from ethanol had m.p. 137°-138°.
Aufarbeitung
- temperaturewarmed at 55°-60° for 40 minutes
- customThe phosphoryl chloride was removed under reduced pressure at 50°
- additionthe residual oil was poured on to ice (200 g)
- filtrationwas filtered