反应详情

温度

70 °C

To a 40 ml DMF solution of ethyl 7-hydroxy-chromane-2-carboxylate (1.81 g, 8.15 mmol) and 3-bromopropyl 2-chloro-4-(2,2,2-trifluoroethoxy)phenyl ether (3.4 g, 9.8 mmol) was added cesium carbonate (3.2 g, 9.8 mmol). The resulting suspension was heated to 70° C. for 5 hr. The solvent was removed under reduced pressure. The residue was diluted with AcOEt and 2N hydrochloric acid. The organic layer was separated, and the aqueous layer was extracted twice with AcOEt. The combined organic layers were dried over anhydrous Na2SO4, filtered, concentrated, and chromatographed on slica gel eluting with 20% AcOEt/hexanes to give the title compound 3.23 g (81%).

1. customThe solvent was removed under reduced pressure
2. additionThe residue was diluted with AcOEt and 2N hydrochloric acid
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted twice with AcOEt
5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customchromatographed on slica gel
9. washeluting with 20% AcOEt/hexanes