反应详情

温度

80 °C

To a suspension of 1-benzyl-N-(1,4-dioxaspiro[4.5]dec-8-yl)-1H-pyrazol-5-amine (38 g) and palladium hydroxide (10 wt %, 11.4 g) in ethanol (200 mL)-acetic acid (40 mL) was added ammonium formate (32 g) by small portions at 80° C. After stirring at 80° C. for 4 hr, the mixture was allowed to cool to room temperature, ethyl acetate was added, and the insoluble material was filtered off. Saturated aqueous sodium hydrogen carbonate was added to the filtrate, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate, and concentrated. The residue was crystallized using ethyl acetate, and the resulting solid was collected by filtration, washed with diisopropyl ether, and dried under reduced pressure to give the title compound as a pale-yellow solid (22 g, 82%).

1. temperatureto cool to room temperature
2. filtrationthe insoluble material was filtered off
3. additionSaturated aqueous sodium hydrogen carbonate was added to the filtrate
4. extractionthe mixture was extracted with ethyl acetate
5. washThe organic layer was washed with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated
8. customThe residue was crystallized
9. filtrationthe resulting solid was collected by filtration
10. washwashed with diisopropyl ether
11. customdried under reduced pressure