反应详情

A solution of 7-(2-(1-methylpiperidin-4-yl)ethoxy)-6-methoxy-3,4-dihydroquinazolin-4-one (3.1 g, 9.8 mmol) in thionyl chloride (40 ml) containing DMF (400 μl) was refluxed for 4 hours. After cooling, the volatiles were removed under vacuum. The residue was partitioned between methylene chloride and water and the pH of the aqueous layer was adjusted to 11 with solid sodium hydrogen carbonate and aqueous ammonia. The organic layer was separated, dried (MgSO4) and evaporated. The residue was triturated with ether, filtered, washed with ether and dried under vacuum to give 4-chloro-6-methoxy-7-(2-(1-methylpiperidin-4-yl)ethoxy)quinazoline (1.83 g, 54%).

1. temperaturewas refluxed for 4 hours
2. temperatureAfter cooling
3. customthe volatiles were removed under vacuum
4. customThe residue was partitioned between methylene chloride and water
5. customThe organic layer was separated
6. dry with materialdried (MgSO4)
7. customevaporated
8. customThe residue was triturated with ether
9. filtrationfiltered
10. washwashed with ether
11. customdried under vacuum