2-chloro-benzoic acid N'-(5-bromo-pyridin-2-yl)hydrazide → 6-Bromo-3-(2-chlorophenyl)-[1,2,4]triazolo[4,3-a]pyridine
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][NH:9][C:10](=O)[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])=[N:6][CH:7]=1>O=P(Cl)(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])=[N:9][N:8]=2)[CH:7]=1Komponenten
3
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 85 °C
Versuchsvorschrift
A mixture of 2-chloro-benzoic acid N′-(5-bromo-pyridin-2-yl)hydrazide (2.96 g, 9.1 mmol) in POCl3 (15 mL) was heated at 85° C. for 48 hours. The solvent was removed in vacuo, and the residue quenched with saturated Na2CO3 and EtOAc. The layers were separated, and the organic layer concentrated in vacuo to minimal volume. The resulting solid was filtered and purified by flash chromatography to give the title compound (0.85 g, 30%).
Aufarbeitung
- customThe solvent was removed in vacuo
- customthe residue quenched with saturated Na2CO3 and EtOAc
- customThe layers were separated
- concentrationthe organic layer concentrated in vacuo to minimal volume
- filtrationThe resulting solid was filtered
- custompurified by flash chromatography
Quellen und Nachweise
- ORD-Eintrag
- ord-e69de3ba1c004d21b1ba54520bbbb072
- Quelldatensatz
- uspto-grants-2008_01
- Patentnummer
- US07321040B2
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