反应详情

温度

100 °C

A mixture of the crude 7-benzyloxy-4-chloro-6-methoxyquinazoline, potassium carbonate (50 g, 362 mmol) and 4-chloro-2-fluorophenol (8.8 ml, 83 mmol) in DMF (500 ml) was stirred at 100° C. for 5 hours then allowed to cool to ambient temperature overnight. The reaction mixture was poured into water (2 l) and was stirred at ambient temperature for a few minutes. The crude solid was collected by filtration washing with water. The resultant solid was dissolved in dichloromethane and filtered through diatomaceous earth. The filtrate was treated with decolourising charcoal, boiled for a few minutes then filtered through diatomaceous earth. The filtrate was filtered through phase separating paper and then evaporated under vacuum to give a solid residue which was triturated with ether, filtered and dried to give 7-benzyloxy-4-(4-chloro-2-fluorophenoxy)-6-methoxyquinazoline (23.2 g, 76%).

1. temperatureto cool to ambient temperature overnight
2. stirringwas stirred at ambient temperature for a few minutes
3. filtrationThe crude solid was collected by filtration
4. washwashing with water
5. dissolutionThe resultant solid was dissolved in dichloromethane
6. filtrationfiltered through diatomaceous earth
7. additionThe filtrate was treated with decolourising charcoal
8. waitboiled for a few minutes
9. filtrationthen filtered through diatomaceous earth
10. filtrationThe filtrate was filtered through phase
11. customseparating paper
12. customevaporated under vacuum
13. customto give a solid residue which
14. customwas triturated with ether
15. filtrationfiltered
16. customdried