Acetic Anhydride → HCID 136199666, Verbindung
Reaktionsgleichung
[C:1]1([C:7]2[N:8]=[C:9]([C:12]3[CH:13]=[N+:14]([O-])[CH:15]=[CH:16][CH:17]=3)[S:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(OC(=O)C)(=[O:21])C>>[O:21]=[C:13]1[C:12]([C:9]2[S:10][CH:11]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[N:8]=2)=[CH:17][CH:16]=[CH:15][NH:14]1Komponenten
3
Versuchsvorschrift
In 25 ml of acetic anhydride was dissolved 2.8 g of 3-(4-phenylthiazol-2-yl)pyridine-N-oxide. The solution was refluxed for 6 hours with heating. The solvent was removed by distillation. The residue was treated with ammonia water and extracted with dichloromethane. The extract was water-washed, dried and subjected to solvent removal by distillation. The residue was mixed with a small amount of dichloromethane. The resulting crystals were collected by filtration and recrystallized from methanol to obtain 60 mg of 2-(2-oxopyridin-3-yl)4-phenylthiazole as light brown plate crystals.
Aufarbeitung
- temperatureThe solution was refluxed for 6 hours
- temperaturewith heating
- customThe solvent was removed by distillation
- additionThe residue was treated with ammonia water
- extractionextracted with dichloromethane
- washwashed
- customdried
- customsubjected to solvent removal by distillation
- additionThe residue was mixed with a small amount of dichloromethane
- filtrationThe resulting crystals were collected by filtration
- customrecrystallized from methanol
Quellen und Nachweise
- ORD-Eintrag
- ord-73c30495b0e04decaaba7f3486db3ed1
- Quelldatensatz
- uspto-grants-1997_10
- Patentnummer
- US05677319
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