反应详情

DMF (0.5 ml) was added to a mixture of 6-methoxy-7-(2-methoxyethoxy)-3,4-dihydroquinazolin-4-one (5.1 g, 20 mmol) in thionyl chloride (50 ml). The mixture was stirred and heated at reflux for 3 hours, allowed to cool and the excess thionyl chloride removed by evaporation. The residue was suspended in methylene chloride and washed with aqueous sodium hydrogen carbonate solution. The aqueous phase was extracted with methylene chloride and the combined extracts dried (MgSO4). The crude product was recrystallised from methylene chloride/hexane to give 4-chloro-6-methoxy-7-(2-methoxyethoxy)quinazoline (2.8 g, 51%) as a fine white solid.

1. temperatureheated
2. temperatureat reflux for 3 hours
3. temperatureto cool
4. customthe excess thionyl chloride removed by evaporation
5. washwashed with aqueous sodium hydrogen carbonate solution
6. extractionThe aqueous phase was extracted with methylene chloride
7. dry with materialthe combined extracts dried (MgSO4)
8. customThe crude product was recrystallised from methylene chloride/hexane