反应详情

温度

90 °C

To 17.5 g of 2,2-dimethyl-N-(3-methylpyridin-4-yl)propionamide, 70 mL of 5N hydrochloric acid aqueous solution was added and stirred at 90° C. for a day. Under ice cooling, the solution was neutralized with 5N sodium hydroxide aqueous solution, and the solvent was evaporated. The crystals were washed with a mixed solution of dichloromethane:methanol=10:1, and the solvent of filtrate was evaporated. To a solution of the resultant crude product in 100 mL of pyridine, 17.2 mL of acetic anhydride was added at room temperature and stirred at this temperature for 6 hours. The solvent was evaporated, and the residue was purified and separated by NH silica gel column chromatography (ethyl acetate:n-hexane=1:1), to afford 12.1 g of the title compound as colorless crystals.

1. customthe solvent was evaporated
2. washThe crystals were washed with a mixed solution of dichloromethane
3. custommethanol=10:1, and the solvent of filtrate was evaporated
4. additionTo a solution of the resultant crude product in 100 mL of pyridine, 17.2 mL of acetic anhydride was added at room temperature
5. stirringstirred at this temperature for 6 hours
6. customThe solvent was evaporated
7. customthe residue was purified
8. customseparated by NH silica gel column chromatography (ethyl acetate:n-hexane=1:1)