m-Chloroperbenzoic acid → 6-Methylpyridine-3-carbonitrile 1-oxide
Reaktionsgleichung
[CH3:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][N:3]=1.ClC1C=CC=C(C(OO)=[O:18])C=1>ClCCl>[C:6]([C:5]1[CH:8]=[CH:9][C:2]([CH3:1])=[N+:3]([O-:18])[CH:4]=1)#[N:7]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A mixture of 6-methylnicotinonitrile (4.15 g) and 3-chloroperbenzoic acid (8.3 g) in dichloromethane (200 ml) was stirred under an argon atomosphere at room temperature for 16h. The dichloromethane was evaporated under reduced pressure and the residue purified by flash column chromatography on silica (K60), using ethyl acetate and then methanol: dichloromethane (1:9 by volume) as eluting solvent to give 5-cyano-2-methylpyridine-1-oxide, mp 133.5°.
Aufarbeitung
- customThe dichloromethane was evaporated under reduced pressure
- customthe residue purified by flash column chromatography on silica (K60)
- washmethanol: dichloromethane (1:9 by volume) as eluting solvent
Quellen und Nachweise
- ORD-Eintrag
- ord-a78378da87434bf7a8573388e582ea7e
- Quelldatensatz
- uspto-grants-1991_03
- Patentnummer
- US04999364
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