反应详情

1-(3,5-Dimethylpyridin-2-yl)piperazine (2.87 g) described in Preparation Example 47 was dissolved in N,N-dimethylformamide (38 ml), 4-bromo-3-fluorobenzoic acid (3.29 g), 1-hydroxybenzotriazole 1 hydrate (2.43 g) and 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide hydrochloride (3.45 g) were added, and the mixture was stirred at room temperature for 4 hr. The reaction mixture was poured into water under cooling, and 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, ethyl acetate and hexane were added and the mixture was stirred at room temperature. The solid was collected by filtration and dried under reduced pressure to give the title compound (3.97 g).

1. temperatureunder cooling
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed twice with water
4. washwashed with saturated brine
5. dry with materialdried over sodium sulfate
6. customThe solvent was evaporated under reduced pressure
7. customthe residue was purified by column chromatography (ethyl acetate:hexane)
8. additionThen, ethyl acetate and hexane were added
9. stirringthe mixture was stirred at room temperature
10. filtrationThe solid was collected by filtration
11. customdried under reduced pressure