反应详情

4-Methyl-(2H)-phthalazin-1-one (6 g) and sodium hydride (1.5 g, 60% in oil) in dimethylformamide (DMF) were stirred at room temperature until hydrogen evolution ceased. To this suspension was added a five fold excess of 1,2-dibromoethane (25 ml) and stirring was continued for a further 2 hours. The solvent was removed and the residue taken up in ethyl acetate, washed twice with brine, dried (MgSO4) and evaporated. Chromatography on silica [Merck `Kieselgel 60` (Trade Mark)] eluting with methylene chloride containing methanol (0% up to 5%) gave, after collection and evaporation of appropriate fractions, a solid which was recrystallised from ethanol to give the title compound, yield 6.25 g, m.p. 102°-103°, used in the next stage.

1. customThe solvent was removed
2. washwashed twice with brine
3. dry with materialdried (MgSO4)
4. customevaporated
5. washChromatography on silica [Merck `Kieselgel 60` (Trade Mark)] eluting with methylene chloride
6. additioncontaining methanol (0% up to 5%)
7. customgave
8. customafter collection and evaporation of appropriate fractions
9. customa solid which was recrystallised from ethanol