反应详情

温度

60 °C

tert-Butyl 4-((methylsulfonyl)oxy)piperidine-1-carboxylate described in Production Example 13-1 (2.7 g, 9.67 mmol) and commercially available ethyl 4-pyrazole carboxylate (1.49 g, 10.6 mmol) were dissolved in N,N-dimethylformamide (30 mL), 50-72% oily sodium hydride (570 mg) was added at 0° C., and the mixture was heated and stirred at 60° C. for 11 hours. The reaction mixture was cooled to room temperature and water and ethyl acetate were added for partition. The organic layer was washed with water twice and then dried over anhydrous sodium sulfate and filtered. The solvent was evaporated, the resultant residue was dissolved in dichloromethane, the resultant was purified with silica gel column chromatography (n-heptane:ethyl acetate=4:1-1:1-1:3-0:1), and the target fraction was concentrated under vacuum to obtain the title compound (2.11 g, 68%).

1. temperaturethe mixture was heated
2. temperatureThe reaction mixture was cooled to room temperature
3. customfor partition
4. washThe organic layer was washed with water twice
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. customThe solvent was evaporated
8. dissolutionthe resultant residue was dissolved in dichloromethane
9. customthe resultant was purified with silica gel column chromatography (n-heptane:ethyl acetate=4:1-1:1-1:3-0:1)
10. concentrationthe target fraction was concentrated under vacuum