反应详情

A mixture of ethyl (3-hydrazinophenyl)acetate (8.77 g, 0.028 mol, available from Example A5) and 4,4,4-trifluoro-3-oxo-butyronitrile (5.75 g, 0.042 mol) in EtOH (200 mL) was heated at reflux overnight. The mixture was concentrated and the residue purified by column chromatography to yield ethyl 2-(3-(5-amino-3-(trifluoromethyl)-1H-pyrazol-1-yl)phenyl)acetate (5 g, 57% yield) as a yellow oil. 1H NMR (300 MHz, DMSO-d6): 7.50-7.43 (m, 3H), 7.30-7.33 (m, 1H), 5.81 (s, 1H), 5.75 (s, 2H), 4.09 (q, J=7.2 Hz, 1H), 3.76 (s, 2H), 3.38 (s, 2H), 1.18 (t, J=7.2 Hz, 3H); MS (ESI) m/z: 314 (M+H+).

1. temperaturewas heated
2. temperatureat reflux overnight
3. concentrationThe mixture was concentrated
4. customthe residue purified by column chromatography