Phosphorus oxychloride → 3-(p-Bromophenyl)-6-chloro-4-methylpyridazine
Reaktionsgleichung
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([CH3:15])=[CH:10][C:11](=O)[NH:12][N:13]=2)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:18])=O>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([Cl:18])=[CH:10][C:9]=2[CH3:15])=[CH:4][CH:3]=1Komponenten
3
Versuchsvorschrift
A 2.0 g. portion of 6-(p-bromophenyl)-5-methyl-3(2H)-pyridazinone and 20 ml. of phosphorus oxychloride are heated on a steam bath for 3 hours. The reaction mixture is poured slowly into crushed ice. The excess phosphorus oxychloride is decomposed. The solid which forms is recovered by filtration, washed with water, dried and recrystallized twice from chloroform, yielding 6-(p-bromophenyl)-5-methyl-3-chloropyridazine, m.p. 197°-200° C.
Aufarbeitung
- additionThe reaction mixture is poured slowly
- custominto crushed ice
- filtrationThe solid which forms is recovered by filtration
- washwashed with water
- customdried
- customrecrystallized twice from chloroform
Quellen und Nachweise
- ORD-Eintrag
- ord-7e7c0c4026c44048b47fb1c593e43e72
- Quelldatensatz
- uspto-grants-1978_05
- Patentnummer
- US04092311
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