反应详情

3-(3-Methyl-5-nitropyrid-2-yl)-3,3-bis(carbethoxy)propionitrile (29.8 g) was dissolved in methanol (1120 ml), molar sodium hydroxide solution (355 ml) was added, the reaction was cooled from 28° C. to room temperature and stirred for 55 minutes. The pH was lowered to 4 by the addition of concentrated hydrochloric acid, the reaction was stirred for 2.75 hr., the pH was then raised to 7 and the methanol was distilled off. The aqueous phase was extracted with chloroform, extracts were dried, filtered and concentrated. The residue was crystallised from chloroform/petroleum ether 40°-60° C. The crude product was treated with charcoal in ethanol and recrystallised from ethanol to give the title compound 10.44 g, m.p. 73°-74° C.

1. temperaturethe reaction was cooled from 28° C. to room temperature
2. stirringthe reaction was stirred for 2.75 hr
3. temperature, the pH was then raised to 7
4. distillationthe methanol was distilled off
5. extractionThe aqueous phase was extracted with chloroform, extracts
6. customwere dried
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was crystallised from chloroform/petroleum ether 40°-60° C
10. additionThe crude product was treated with charcoal in ethanol
11. customrecrystallised from ethanol