反应详情

温度

100 °C

To a solution of 4-chloro-6-methoxy-7-((1-(2-methylsulphonylethyl)piperidin-4-yl)methoxy)quinazoline (115 mg, 0.28 mmol) and 7-hydroxyquinoline (50 mg, 0.33 mmol) in DMF (1.5 ml) was added potassium carbonate (60 mg, 0.42 mmol). The mixture was stirred for 2 hours at 100° C. After cooling, and removal of the volatiles by evaporation, the residue was partitioned between ethyl acetate and water. The organic layer was washed with water, brine, dried (MgSO4) and evaporated. The residue was purified by column chromatography eluting with ethylacetate/methylene chloride/methanol (1/1/0 followed by 40/50/10 and 0/9/1). After removal of the volatiles by evaporation, the residue was triturated with pentane, filtered and dried under vacuum to give 6-methoxy-7-((1-(2-methylsulphonylethyl)piperidin-4-yl)methoxy)-4-(quinolin-7-yloxy)quinazoline (110 mg, 76%).

1. temperatureAfter cooling
2. customremoval of the volatiles
3. customby evaporation
4. customthe residue was partitioned between ethyl acetate and water
5. washThe organic layer was washed with water, brine
6. dry with materialdried (MgSO4)
7. customevaporated
8. customThe residue was purified by column chromatography
9. washeluting with ethylacetate/methylene chloride/methanol (1/1/0 followed by 40/50/10 and 0/9/1)
10. customAfter removal of the volatiles
11. customby evaporation
12. customthe residue was triturated with pentane
13. filtrationfiltered
14. customdried under vacuum