반응 #82457

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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

수율 70.0%

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후처리

1. 1
   기타the product is obtained as a precipitate
2. 2
   여과is filtered
3. 3
   세척washed with hexane
4. 4
   기타to yield 23.4 g, 70% yield
5. 5
   기타of solid which is recrystallized from isopropanol
6. 6
   기타to give a pure product, melting point 182°-183° C.

실험 절차

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.

출처