反应详情

温度

23 °C

A mixture of 7-cyclopropyl-5-(4-trifluoromethyl-phenyl)-pyrazolo[1,5-a]pyridine-3-carboxylic acid (example C.28 step 6) (1.03 g, 2.97 mmol) in acetic acid (40 mL) was refluxed for 20 h. Cooled to 23° C., added NaOAc (325 mg, 3.95 mmol) and ICl (2M in HOAc, 1.85 mL, 3.7 mmol) and the mixture was stirred at 23° C. for 2 h. Poured into water, filtered precipitate off, washed with water, dissolved in TBME, washed with sat. NaHCO3-sol.+little sat. Na2SO3-sol. and brine, dried over Na2SO4. Removal of the solvent in vacuum left the title compound as a light red solid (1.257 g, 99%). MS (ISP) 429.2 [(M+H)+].

1. temperaturewas refluxed for 20 h
2. filtrationfiltered precipitate off,
3. washwashed with water
4. dissolutiondissolved in TBME
5. washwashed with sat. NaHCO3-sol
6. dry with materialand brine, dried over Na2SO4
7. customRemoval of the solvent in vacuum
8. waitleft the title compound as a light red solid (1.257 g, 99%)