反应详情

温度

70 °C

To a 2 ml DMF solution of ethyl 7-(3-bromopropoxy)-2-ethylchromane-2-carboxylate (40 mg, 0.108 mmol) and 3-trifluoromethyl-7-propyl-6-hydroxybenzisoxazole (U.S. Pat. No. 6,090,836) (29 mg, 0.118 mmol) was added cesium carbonate (39 mg, 0.12 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 water. 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 silica gel. Elution with 20% AcOEt/hexanes gave the title compound as a pale yellow oil 49 mg (85%).

1. customThe solvent was removed under reduced pressure
2. additionThe residue was diluted with AcOEt and water
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 silica gel
9. washElution with 20% AcOEt/hexanes