反应详情

76 mg of sodium hydride (80% in mineral oil) are added to a suspension of 400 mg of 6-hydroxy-3H-quinazolin-4-one in 20 ml of dry dimethylformamide. After stirring for 30 minutes at room temperature, 560 mg of 2,6-dimethoxybenzylbromide are added, and stirring is continued overnight. The solvent is distilled off in vacuo, and the residue partitioned between aqueous pH7-buffer solution and ethyl acetate. The organic phase is separated, dried over magnesium sulfate and evaporated in vacuo. Silica gel chromatography yields a minor amount of the N,O-bis-alkylated product followed by the pure title compound as colourless crystals. mp: 243-245°.

1. stirringstirring
2. waitis continued overnight
3. distillationThe solvent is distilled off in vacuo
4. customthe residue partitioned between aqueous pH7-buffer solution and ethyl acetate
5. customThe organic phase is separated
6. dry with materialdried over magnesium sulfate
7. customevaporated in vacuo
8. customSilica gel chromatography yields a minor amount of the N,O-bis-alkylated product