反应详情

2-Amino-5-chloropyridine (179 mg) is dissolved in chloroform (5 ml), and there to is added dropwise 0.98 M trimethyl aluminum-hexane solution (1.42 ml) under ice-cooling. The reaction solution is stirred at room temperature for 0.5 hours, and thereto is added methyl 3-({[trans-4-(3-oxomorpholin-4-yl)cyclohexyl]carbonyl}amino)-thiophene-2-carboxylate (170 mg), and the mixture is heated to reflux for 18 hours. After allowing to cool, to the reaction mixture is added 10% hydrochloric acid (4 ml), and the mixture is extracted with chloroform. The organic layer is washed successively with water and saturated brine, dried over sodium sulfate, and evaporated to remove the solvent under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (eluent: chloroform) to give the title compound (172 mg). APCI-MS M/Z: 463/465[M+H]+

1. temperaturecooling
2. temperaturethe mixture is heated
3. temperatureto reflux for 18 hours
4. temperatureto cool, to the reaction mixture
5. extractionthe mixture is extracted with chloroform
6. washThe organic layer is washed successively with water and saturated brine
7. dry with materialdried over sodium sulfate
8. customevaporated
9. customto remove the solvent under reduced pressure
10. customThe resulting residue is purified by NH-silica gel column chromatography (eluent: chloroform)