Reaktionsgleichung
[CH3:1][C:2]1[C:3]([C:8]([OH:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.[ClH:11]>CCO.O.O=[Pt]=O>[ClH:11].[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][NH:4][CH:3]1[C:8]([OH:10])=[O:9]Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
3-Methylpicolinic acid (50 g, 365 mmol) was dissolved in 400 mL of EtOH:H2O (1:1) with 60 mL of aq. HCl (32%). PtO2 (5 g) was then added and the reaction stirred at rt under a hydrogen balloon until NMR indicated completion. The reaction was filtered through diatomaceous earth and concentrated to yield the title compound as a white solid which was used without further purification (60.5 g, 92%). 1H NMR (MeOD, 400 MHz) δ 4.13-4.11 (m, 1H), 3.40-3.33 (m, 1H), 3.05-2.99 (m, 1H), 2.61-2.58 (m, 1H), 1.92-1.72 (m, 4H), 1.09 (d, J=7.0 Hz, 3H). MS (ESI) 452.16 (M+H).
Aufarbeitung
- filtrationThe reaction was filtered through diatomaceous earth
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-8dd168f0ae5b41038fb0efec3c341930
- Quelldatensatz
- uspto-grants-2016_09
- Patentnummer
- US09440982B2
Verknüpfte Notizen
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