反应详情

To a mixture of 3-{[5-(morpholin-4-ylcarbonyl)-4-(trifluoromethyl)pyrimidin-2-yl]amino}adamantan-1-ol (150 mg) and dichloromethane (3 mL) was added diethylaminosulfur trifluoride (70 μL) under ice-cooling, followed by stirring at room temperature for 30 minutes. The reaction mixture was alkalified by adding a saturated aqueous sodium hydrogen carbonate solution, and the aqueous layer was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate) to obtain N-(3-fluoroadamantan-1-yl)-5-(morpholin-4-ylcarbonyl)-4-(trifluoromethyl)pyrimidin-2-amine (115 mg) as a white solid.

1. temperaturecooling
2. extractionthe aqueous layer was extracted with ethyl acetate
3. washThe organic layer was washed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe obtained residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate)