反应详情

温度

100 °C

A mixture of [4-(5-cyclopropyl-3-methylpyridin-2-yl)piperazin-1-yl](6-fluoro-4-methylpyridin-3-yl)methanone (1.45 g) described in Preparation Example 140 and 4-methoxybenzylamine (1.12 g) was stirred at 100° C. for 5 hr. The reaction mixture was cooled, water was added, and the mixture was extracted with chloroform. The organic layer was washed with saturated brine, and the solvent was evaporated. The obtained residue was dissolved in dichloromethane (10 mL), trifluoroacetic acid (20 mL) was added, and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture, and the mixture was extracted with dichloromethane. The organic layer was washed with saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate) to give the title compound (1.07 g).

1. temperatureThe reaction mixture was cooled
2. extractionthe mixture was extracted with chloroform
3. washThe organic layer was washed with saturated brine
4. customthe solvent was evaporated
5. dissolutionThe obtained residue was dissolved in dichloromethane (10 mL)
6. additiontrifluoroacetic acid (20 mL) was added
7. stirringthe mixture was stirred at room temperature overnight
8. additionWater was added to the reaction mixture
9. extractionthe mixture was extracted with dichloromethane
10. washThe organic layer was washed with saturated brine
11. customthe solvent was evaporated
12. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate)