反应详情

A mixture of 4-chloro-1-(2,4-dimethylphenyl)-1,6-dihydro-7H-pyrrolo[2,3-d]pyridazin-7-one (0.30 g, 1.10 mmol), MeI (0.075 ml, 1.21 mmol), potassium carbonate (0.30 g, 2.2 mmol) and DMF (5 ml) was stirred at room temperature for 13 hours. The mixture was diluted with water (50 ml) and extracted with ethyl acetate (50 ml×2). The extracts were combined, washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with hexane/ethyl acetate (5:1) to give 0.31 g (98%) of the title compound as crystals.

1. extractionextracted with ethyl acetate (50 ml×2)
2. washwashed with water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was purified by silica gel chromatography
6. washeluting with hexane/ethyl acetate (5:1)