反应详情

温度

150 °C

A mixture of 4,6-dichloro-2-methylpyridazin-3(2H)-one (5.0 g, 27.9 mmol) and ammonium hydroxide (55 mL, 1412 mmol) was heated at 150° C. for 2 hours and then cooled to room temperature. The solvent was removed, and the residue was dissolved in ethyl acetate and washed with water. The aqueous layer was extracted with additional ethyl acetate three times. The combined organic layers were washed with brine, dried and concentrated. The residue was purified by flash chromatography (silica gel, eluted with 40% ethyl acetate in hexanes to afford 3.85 g (87%) of the title compound.

1. temperaturecooled to room temperature
2. customThe solvent was removed
3. dissolutionthe residue was dissolved in ethyl acetate
4. washwashed with water
5. extractionThe aqueous layer was extracted with additional ethyl acetate three times
6. washThe combined organic layers were washed with brine
7. customdried
8. concentrationconcentrated
9. customThe residue was purified by flash chromatography (silica gel
10. washeluted with 40% ethyl acetate in hexanes