反应详情

Phenol (29.05 g, 309 mmol) was dissolved in NMP (210 ml), sodium hydride (11.025 g, 60% dispersion in mineral oil) was added in portions with cooling and the mixture was stirred for 3 hours. The viscous suspension was diluted with NMP (180 ml) and stirred overnight. The solution of 7-benzyloxy-4-chloro-6-methoxyquinazoline was added and the suspension stirred at 100° C. for 2.5 hours. The suspension was allowed to cool to ambient temperature and poured into water (1.5 l) with vigorous stirring. The precipitate was collected by filtration, washed with water and dried under vacuum. The residue was dissolved in dichloromethane, washed with brine and filtered through phase separating paper. The filtrate was evaporated under vacuum then triturated with ether to give 7-benzyloxy-6-methoxy-4-phenoxyquinazoline (87.8 g, 83%) as a pale cream solid.

1. temperaturewith cooling
2. stirringstirred overnight
3. stirringthe suspension stirred at 100° C. for 2.5 hours
4. filtrationThe precipitate was collected by filtration
5. washwashed with water
6. customdried under vacuum
7. dissolutionThe residue was dissolved in dichloromethane
8. washwashed with brine
9. filtrationfiltered through phase
10. customseparating paper
11. customThe filtrate was evaporated under vacuum
12. customthen triturated with ether