反应详情

To 1.1 g (5.52 mmol) of 3-oxo-3-(2,3,6-trifluorophenyl)propanenitrile diluted in 20 ml of acetonitrile are respectively added 1.60 g (5.52 mmol) of tert-butyl 4-(4-formylphenyl)piperazine-1-carboxylate and 0.53 g (5.52 mmol) of 3-amino-5-methyl-pyrazole. The reaction mixture is refluxed for 4 h then the solvent is concentrated. The residue is purified by chromatography on silica (cyclohexane/ethyl acetate eluent: 5:5) then the solid obtained is triturated in ethyl acetate and dried to yield 2.48 g (81%) of tert-butyl 4-(4-(5-cyano-3-methyl-6-(2,3,6-trifluorophenyl)-4,7-dihydro-1H-pyrazolo[3,4-b]pyridin-4-yl)phenyl)piperazine-1-carboxylate in the form of a yellow solid.

1. temperatureThe reaction mixture is refluxed for 4 h
2. concentrationthe solvent is concentrated
3. customThe residue is purified by chromatography on silica (cyclohexane/ethyl acetate eluent: 5:5)
4. customthe solid obtained
5. customis triturated in ethyl acetate
6. customdried