反应详情

To methyl 5-[2-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)ethyl]-2-(propan-2-yloxy)pyridine-4-carboxylate (112c, 0.630 g, 1.71 mmol) in EtOH (50 mL) was added hydrazine monohydrate (0.850 mL, 17.1 mmol). The reaction mixture was refluxed for 5 hours. The reaction mixture was cooled to room temperature and the white solids collected by filtration and rinsed with EtOH. The mother liquor was concentrated and H2O (25 mL) was added, then the aqueous layer extracted with EtOAc (3×25 mL) The combined organic layers were concentrated under vacuum and purified by column chromatography (0-80% ethyl acetate/heptanes) to give 7-(propan-2-yloxy)-3,4-dihydro-2,6-naphthyridin-1(2H)-one (112d, 337 mg, 96%) as a white solid.

1. temperatureThe reaction mixture was refluxed for 5 hours
2. filtrationthe white solids collected by filtration
3. washrinsed with EtOH
4. concentrationThe mother liquor was concentrated
5. additionH2O (25 mL) was added
6. extractionthe aqueous layer extracted with EtOAc (3×25 mL) The combined organic layers
7. concentrationwere concentrated under vacuum
8. custompurified by column chromatography (0-80% ethyl acetate/heptanes)