反应详情

To a clear solution of (7-cyano-pyrazolo[1,5-a]pyridin-4-yl)-carbamic acid tert-butyl ester (3 g, 11.6 mmol) in methylene chloride (40 mL) was added TFA (8 mL). The mixture was stirred at rt for 3 h, and then concentrated under reduced pressure. The residue was partitioned between EtOAc (100 mL) and sat. NaHCO3 solution (50 mL). The aqueous solution was separated and extracted with EtOAc (2×50 mL). The combined organic solutions were dried over Na2SO4, filtered though SiO2 pad, and concentrated under reduced pressure. Crystallization in EtOAc and 95% EtOH gave compound 777F (1.07 g, 58%) as a dark yellow solid. HPLC: 97% at 1.96 min (retention time) (YMC S5 ODS-A column 4.6×50 mm eluting with 10-90% aqueous methanol over 4 mincontaining 0.2% phosphoric acid, 4 mL/min, monitoring at 220 nm). MS (ES): m/z 159 [M+H]+.

1. concentrationconcentrated under reduced pressure
2. customThe residue was partitioned between EtOAc (100 mL) and sat. NaHCO3 solution (50 mL)
3. customThe aqueous solution was separated
4. extractionextracted with EtOAc (2×50 mL)
5. dry with materialThe combined organic solutions were dried over Na2SO4
6. filtrationfiltered though SiO2 pad
7. concentrationconcentrated under reduced pressure
8. customCrystallization in EtOAc