反应详情

A mixture of methyl 6-oxo-3,4-diphenyl-1(6H)-pyridazinenonanoate (6 g, 14 mmol), 5N NaOH solution (8.6 mL, 43 mmol) and methanol (100 mL) was heated to reflux on a steam bath. After 30 minutes, the mixture was concentrated, diluted with water and acidified to pH=1 with 2N HCl solution. The mixture was extracted with CH2Cl2, the combined extracts dried over sodium sulfate and concentrated to leave an oil that crystallized on standing. Recrystallization from a mixture of CH2Cl2 and hexanes gave 6-oxo-3,4-diphenyl-1(6H)-pyridazinenonanoic acid (3.92 g, 67%) mp 100°-103° C.

1. temperaturewas heated
2. temperatureto reflux on a steam bath
3. concentrationthe mixture was concentrated
4. additiondiluted with water
5. extractionThe mixture was extracted with CH2Cl2
6. dry with materialthe combined extracts dried over sodium sulfate
7. concentrationconcentrated
8. customto leave an oil that
9. customcrystallized
10. customRecrystallization
11. additionfrom a mixture of CH2Cl2 and hexanes