反应详情

温度

85 °C

A solution of 6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)-3,4-dihydroquinazolin-4-one (2.8 g, 9.24 mmol) in thionyl chloride (28 ml) containing DMF (280 μl) was heated at reflux at 85° C. for 1 hour. After cooling, the volatiles were removed by evaporation. The precipitate was triturated with ether, filtered, washed with ether and dried under vacuum. The solid was dissolved in methylene chloride and saturated aqueous sodium hydrogen carbonate was added. The organic layer was separated, washed with water, brine, dried (MgSO4) and evaporated to give 4-chloro-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline (2.9 g, 98%).

1. temperaturewas heated
2. temperatureAfter cooling
3. customthe volatiles were removed by evaporation
4. customThe precipitate was triturated with ether
5. filtrationfiltered
6. washwashed with ether
7. customdried under vacuum
8. dissolutionThe solid was dissolved in methylene chloride
9. additionsaturated aqueous sodium hydrogen carbonate was added
10. customThe organic layer was separated
11. washwashed with water, brine
12. dry with materialdried (MgSO4)
13. customevaporated