反应详情

To a solution of sodium hydride (168 mg, 60% in oil) in N,N-dimethylformamide (10 mL) was added oxazolidin-2-one (367 mg) under ice-cooling, and the mixture was stirred at room temperature. Thereto was added a solution of [4-(3,5-dicyclopropylpyridin-2-yl)piperazin-1-yl](6-fluoro-4-methylpyridin-3-yl)methanone (400 mg) described in Preparation Example 139 in N,N-dimethylformamide (5 mL) and the mixture was stirred at 90° C. for 5 hr. Water was poured into the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed twice with water, washed with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by column chromatography (ethyl acetate:hexane). Then, diethyl ether was added and the mixture was stirred at room temperature. The solid was collected by filtration to give the title compound (215 mg).

1. temperaturecooling
2. stirringthe mixture was stirred at 90° C. for 5 hr
3. extractionthe mixture was extracted with ethyl acetate
4. washThe organic layer was washed twice with water
5. washwashed with saturated brine
6. dry with materialdried over sodium sulfate
7. customThe solvent was evaporated under reduced pressure
8. customthe residue was purified by column chromatography (ethyl acetate:hexane)
9. additionThen, diethyl ether was added
10. stirringthe mixture was stirred at room temperature
11. filtrationThe solid was collected by filtration