反应详情

4,5-Dichloro-2-methylpyridazin-3(2H)-one (1 g) is dissolved in aqueous HI solution (57%, 8.5 mL) and the mixture is heated to reflux for 12 hours. After cooling to room temperature the mixture is treated with aqueous Na2S2O3 solution (30%, 100 mL) and stirred for 1 hour. The mixture is then extracted three times with dichloromethane. The combined organic phases are washed with brine, dried (MgSO4) and concentrated. The residue is triturated with diisopropylether. Yield: 414 mg; Mass spectrum (ESI+): m/z=145 [M+H]+.

1. temperaturethe mixture is heated
2. temperatureto reflux for 12 hours
3. extractionThe mixture is then extracted three times with dichloromethane
4. washThe combined organic phases are washed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customThe residue is triturated with diisopropylether