反应详情

Suspend sodium hydride (1.13 g, 47 mmol) in a solution of 6-iodo-3H-quinazolin-4-one (2.5 g, 9.2 mmol) in DMF. Stir at room temperature for 20 min, add iodomethane (6.6 g, 46 mmol) into the mixture and stir for 2 h. Dilute the mixture with 3:1 chloroform/isopropyl alcohol and wash with saturated sodium chloride solution. Dry the organic phase (sodium sulfate) and concentrate in vacuo. Purify the residue with flash chromatography (dichloromethane to dichloromethane/methanol) to give 2.5 g (95%) of the titled compound as a white solid. MS ES+ m/e 287 (M+1).

1. stirringstir for 2 h
2. washwash with saturated sodium chloride solution
3. dry with materialDry the organic phase (sodium sulfate)
4. concentrationconcentrate in vacuo
5. customPurify the residue with flash chromatography (dichloromethane to dichloromethane/methanol)