反应详情

To a suspension of 2-(isonicotinoyl)benzoic acid (10.0 g, 44.1 mmol) in toluene (50 mL) was added methyl hydrazine (2.59 mL, 48.6 mmol). The mixture was heated to reflux while collecting water in a Dean-Stark trap for 6 hours. Additional methylhydrazine (2.59 mL) was added and the mixture was heated to reflux for another 5 hours. The reaction mixture was cooled to room temperature and the product was collected by filtration. The product was recrystallized from hot methanol to afford 8.5 g (81%) of 2-methyl-4-(4-pyridyl)-1-(2H)-phthalazinone, m.p. 173°-174° C.

1. temperatureThe mixture was heated
2. temperatureto reflux
3. customwhile collecting water in a Dean-Stark trap for 6 hours
4. additionAdditional methylhydrazine (2.59 mL) was added
5. temperaturethe mixture was heated
6. temperatureto reflux for another 5 hours
7. filtrationthe product was collected by filtration
8. customThe product was recrystallized from hot methanol