反应详情

A solution of 2,6-dihydro-2-methyl-4-(2-methylpropyl)-1H-pyrrolo[3,4-d]pyridazin-1-one (0.65 g) in dry dimethyl formamide (3 ml) was added dropwise to sodium hydride (0.15 g of a 60% dispersion in oil) in dimethyl formamide (10 ml) with stirring. After 20 minutes benzyl bromide (0.45 ml) and a crystal of potassium iodide were added. The mixture was stirred for 11 days and then poured into dilute hydrochloric acid, which was extracted with ethyl acetate. The organic phase was washed with water, dried, and evaporated to give an oil, which was purified by chromatography on silica (ethyl acetate/isohexane 3:1) to afford, after crystallisation from cyclohexane, 2,6-dihydro-2-methyl-4-(2-methylpropyl)-6-phenylmethyl-1H-pyrrolo[3,4-d]pyridazin-1-one (0.3 g).

1. stirringThe mixture was stirred for 11 days
2. extractionwas extracted with ethyl acetate
3. washThe organic phase was washed with water
4. customdried
5. customevaporated
6. customto give an oil, which
7. customwas purified by chromatography on silica (ethyl acetate/isohexane 3:1)
8. customto afford
9. customafter crystallisation from cyclohexane, 2,6-dihydro-2-methyl-4-(2-methylpropyl)-6-phenylmethyl-1H-pyrrolo[3,4-d]pyridazin-1-one (0.3 g)