反应详情

温度

110 °C

To a stirring solution of crude 2-tert-butyl-5-cyclobutyl-2H-pyrazol-3-ylamine (1.0 g, 5.2 mmol) in AcOH (5 mL) was added 3-oxo-2-phenyl-propionic acid ethyl ester (1.0 g, 5.2 mmol). The reaction was then heated to 110° C. for 18 hr, at which time the reaction was cooled to room temperature, concentrated under reduced pressure to remove HOAc, diluted with EtOAc, and quenched with a saturated aqueous solution of NaHCO3. The organic layer was dried over MgSO4, filtered through a fritted funnel, and concentrated under reduced pressure. Purification of the resulting material was accomplished by flash chromatography with a Biotage® 35L column (A Dynax Corp., Charlottesville, Va.), eluting with a gradient of 5%, 10%, 20% EtOAc/hexanes. The product was collected and concentrated under reduced pressure to give the title compound (15 mg, 9% yield). LRMS m/z (APCl) 322 (M+1).

1. temperaturewas cooled to room temperature
2. concentrationconcentrated under reduced pressure
3. customto remove HOAc
4. additiondiluted with EtOAc
5. customquenched with a saturated aqueous solution of NaHCO3
6. dry with materialThe organic layer was dried over MgSO4
7. filtrationfiltered through a fritted funnel
8. concentrationconcentrated under reduced pressure
9. customPurification of the resulting material
10. wash), eluting with a gradient of 5%, 10%, 20% EtOAc/hexanes
11. customThe product was collected
12. concentrationconcentrated under reduced pressure