Phosphorus oxychloride → Dimethyl 4-chloropyridine-3,5-dicarboxylate
Reaktionsgleichung
O=[C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][NH:5][CH:4]=[C:3]1[C:12]([O:14][CH3:15])=[O:13].O=P(Cl)(Cl)[Cl:18]>>[Cl:18][C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][N:5]=[CH:4][C:3]=1[C:12]([O:14][CH3:15])=[O:13]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 140 °C
Versuchsvorschrift
A mixture of dimethyl 4-oxo-1,4-dihydropyridine-3,5-dicarboxylate (3 g, crude) and POCl3 (10 mL) was heated to 140° C. in the sealed tube for 15 hours. The mixture was cooled to RT, poured into ice and extracted with ether. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated to afford the title compound as solid (yield 33.7%).