反应详情

温度

85 °C

A suspension of 2.0 g (8.3 mmol) of 1-benzyl-2-methyl-6,7-dihydropyrrolo[2,3-d]pyridazine 7-one in 20 ml of phosphorus oxychloride is stirred at 85° C. for 7 h. The excess phosphorus oxychloride is subsequently distilled off and the residue is hydrolyzed in 50 ml of water. After neutralization with 2 N sodium hydroxide solution, the mixture is extracted with 3×50 ml of dichloromethane. The organic extracts are washed with 50 ml of water, dried over magnesium sulfate and concentrated. The residue is recrystallized from methanol. 1.8 g (84%) of the title compound are isolated. M.p.: 152°-156° C.

1. distillationThe excess phosphorus oxychloride is subsequently distilled off
2. extractionAfter neutralization with 2 N sodium hydroxide solution, the mixture is extracted with 3×50 ml of dichloromethane
3. washThe organic extracts are washed with 50 ml of water
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customThe residue is recrystallized from methanol