反应详情

温度

80 °C

Trans-3-(4-aminocyclohexylcarbonylamino)-N-(5-chloropyridin-2-yl)benzofuran-2-carboxamide dihydrochloride (200 mg) obtained in Example 219, tetrahydro-2,5-dimethoxyfuran (53 μl), sodium acetate (68 mg) are stirred at 80° C. for 2 hours in acetic acid (3 ml). To the mixture is added tetrahydro-2,5-dimethoxyfuran (26 μl), and the mixture is further stirred at 80° C. for 2 hours. After cooling, the reaction solution is poured into ice-water, and the mixture is extracted with chloroform. The organic layer is washed with a saturated aqueous sodium hydrogen carbonate solution, a saturated brine, and dried over sodium sulfate, and the solvent is evaporated under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (eluent: ethyl acetate/hexane=1/5→ethyl acetate/hexane=1/3) to give the title compound (96 mg).

1. temperatureAfter cooling
2. extractionthe mixture is extracted with chloroform
3. washThe organic layer is washed with a saturated aqueous sodium hydrogen carbonate solution
4. dry with materiala saturated brine, and dried over sodium sulfate
5. customthe solvent is evaporated under reduced pressure
6. customThe resulting residue is purified by NH-silica gel column chromatography (eluent: ethyl acetate/hexane=1/5→ethyl acetate/hexane=1/3)