Reaktionsgleichung
N[C:2]1[CH:9]=[C:8]([CH3:10])[C:5]([C:6]#[N:7])=[C:4]([CH3:11])[N:3]=1.N([O-])=[O:13].[Na+]>S(=O)(=O)(O)O.O>[OH:13][C:2]1[CH:9]=[C:8]([CH3:10])[C:5]([C:6]#[N:7])=[C:4]([CH3:11])[N:3]=1Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
To a stirred solution of 6-amino-2,4-dimethylnicotinonitrile (Sato, K.; et al. Bull. Chem. Soc. Jpn., 1969, 42, 2319., 22.4 g, 152 mmol) in 5% aqueous sulfuric acid (600 mL) was added dropwise a solution of sodium nitrite (25.2 g, 365 mmol) in water (100 mL) at 0° C., and the mixture was stirred at room temperature for 16 h. The resulting precipitate was collected by filtration to afford 10.2 g (45%) of the title compound: 1H-NMR (DMSO-d6) δ 12.27 (1H, br.s), 6.17 (1H, s), 2.38 (3H, s), 2.20 (3H, s).
Aufarbeitung
- filtrationThe resulting precipitate was collected by filtration
Quellen und Nachweise
- ORD-Eintrag
- ord-1a40d4722aa2421c89bec976b94a721f
- Quelldatensatz
- uspto-grants-2011_04
- Patentnummer
- US07928119B2
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