Reaktionsgleichung
[C:1]([NH:4][C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][N:6]=1)(=[O:3])[CH3:2].P([O-])([O-])(O)=O.[Na+].[Na+].[Cl:19]CCl.ClCl>O>[C:1]([NH:4][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([Cl:19])=[CH:7][N:6]=1)(=[O:3])[CH3:2]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
In 300 ml of water, 15.0 g (0.1 mol) of 2-acetamido-4-methylpyridine (Ia) was dissolved. To this solution, 35.5 g (0.25 mol) of disodium hydrogenphosphate and 100 ml of dichloromethane were added in this order. While this mixture was stirred, 8.0 g (0.11 mol) of chlorine was introduced thereto at 0° C. for one hour. After having further been stirred at the same temperature for 2 hours, the mixture was separated into a water layer and an extract layer. After the water layer was further extracted with 100 ml of dichloromethane, the newly-separated extract layer was combined with the previously-separated extract layer and washed with saturated brine. Then the washed mixture was desiccated with sodium sulfate anhydride. When the solvent was evaporated off, 18.0 g (yield: 97.3%) of 2-acetamido-4-methyl-5-chloropyridine (IIk) was obtained as a pale yellow crystal.
Aufarbeitung
- stirringAfter having further been stirred at the same temperature for 2 hours
- customthe mixture was separated into a water layer
- extractionAfter the water layer was further extracted with 100 ml of dichloromethane
- extractionthe newly-separated extract layer
- extractionextract layer
- washwashed with saturated brine
- customWhen the solvent was evaporated off
Quellen und Nachweise
- ORD-Eintrag
- ord-dfea721de0154d2093786bb733e102d8
- Quelldatensatz
- uspto-grants-1995_09
- Patentnummer
- US05453512
Verknüpfte Notizen
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