Formamide → 4-Hydroxypyrido (2,3-d)pyrimidine
Reaktionsgleichung
[NH2:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH:11]([NH2:13])=O>>[N:1]1[C:2]2[N:10]=[CH:9][CH:8]=[CH:7][C:3]=2[C:4](=[O:6])[NH:13][CH:11]=1Komponenten
3
Versuchsvorschrift
2-Amino nicotinic acid (15 g, 108.6 mmol) in formamide (35 mL) is heated to 165 −170° C. for 3.5 h. Upon cooling a solid precipitates. The solid is filtered and washed with H2O and dried in a vacuum oven to give 3H-pyrido[2,3-d]pyrimidin-4-one (7.87 g, 49.4). 1H NMR (DMSO) δ 12.50 (1H, s), 8.97 (1H, dd, J=1.9, 4.5 Hz), 8.53 (1H, dd, J=2.1, 7.9 Hz), 8.34 (1H, s), 7.57 (1H, dd, J=4.6, 8.0 Hz).
Aufarbeitung
- temperatureUpon cooling a solid
- customprecipitates
- filtrationThe solid is filtered
- washwashed with H2O
- customdried in a vacuum oven
Quellen und Nachweise
- ORD-Eintrag
- ord-16466fd53fde427f990b44b3d26336cd
- Quelldatensatz
- uspto-grants-2004_03
- Patentnummer
- US06713484B2
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