Reaktion #82457

Reaktionsgleichung

Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3pyridinedicarboxylate

N,N-dimethylformamide dineopentyl acetal

→

diethyl 5-[3-(dimethylamino)acryloyl]-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate

Ausbeute 70.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe product is obtained as a precipitate
2. 2
   Filtrationis filtered
3. 3
   Waschenwashed with hexane
4. 4
   Sonstigeto yield 23.4 g, 70% yield
5. 5
   Sonstigeof solid which is recrystallized from isopropanol
6. 6
   Sonstigeto give a pure product, melting point 182°-183° C.

Vorschrift

Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3pyridinedicarboxylate, (25 g, 0.089 mol) and N,N-dimethylformamide dineopentyl acetal (50 mL, 98%, 40.62 g, 0.176 mol) are heated for 30 minutes at 80°-100° C. After cooling to room temperature, the product is obtained as a precipitate and is filtered and washed with hexane to yield 23.4 g, 70% yield, of solid which is recrystallized from isopropanol to give a pure product, melting point 182°-183° C.

Quelle