反应详情

温度

180 °C

A mixture of 3-cyclobutyl-7-[(5-iodo-2-pyridinyl)oxy]-2,3,4,5-tetrahydro-1H-3-benzazepine (E207) (294 mg, 0.7 mmol), pyrazole (58 mg, 0.84 mmol), cesium carbonate (479 mg, 1.5 mmol), copper (I) iodide (7 mg, 0.04 mmol) and 1,10 phenanthroline (13 mg, 0.07 mmol) in dioxane (2 ml) were heated in a microwave reactor at 180° C. for 20 minutes. The reaction mixture was diluted with ethyl acetate and washed with a saturated solution of ammonium chloride, water, brine and dried (magnesium sulfate). The organic layer was filtered, concentrated in vacuo and the resulting residue was purified by column chromatography eluting with a mixture of 0.880 ammonia:methanol:dichloromethane (0.5:4.5:95) to afford the title compound (E221); MS (ES+) m/e 361 [M+H]+.

1. washwashed with a saturated solution of ammonium chloride, water, brine
2. dry with materialdried (magnesium sulfate)
3. filtrationThe organic layer was filtered
4. concentrationconcentrated in vacuo
5. customthe resulting residue was purified by column chromatography
6. washeluting with a mixture of 0.880 ammonia:methanol:dichloromethane (0.5:4.5:95)