反应详情

1-{4-[1-(4-Methoxy-phenyl)-7-oxo-3-trifluoromethyl-1,4,5,7-tetrahydro-pyrazolo[3,4-c]pyridin-6-yl]-phenyl}cyclopropane carboxylic acid (1.12 g, 2.37 mmol) and N,O-dimethylhydroxylamine hydrochloride (0.255 g, 2.61 mmol) were dissolved in DMF (20.0 mL) and DIEA (2.0 mL, 11.5 mmol) was added dropwise. 1-[3-(Dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (0.54 g, 2.8 mmol) was added and the reaction was allowed to proceed under nitrogen at rt for 12 h. The reaction was diluted with EtOAc, washed 1N HCl, brine, dried over Na2SO4, filtered and concentrated. The reaction was purified via flash chromatography (silica, 100% EtOAc, then 10% MeOH/CH2Cl2) to give the title compound. LC/MS (ESI+) 515.6 (M+H).

1. washwashed 1N HCl, brine
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe reaction was purified via flash chromatography (silica, 100% EtOAc