反应详情

温度

80 °C

To a solution of 3-(4-methoxyphenyl)-3-oxo-propionitrile (2.0 g, 11.4 mmol) in absolute ethanol (21 mL) was added hydrazine hydrate (3.32 mL, 68.3 mmol). The reaction mixture was stirred at 80° C. for 15 hours, then it was concentrated in vacuo and purified on silica gel with 0-10% MeOH in CH2Cl2 as eluent to give 2.02 g (97% yield) of 5-amino-3-(4-methoxyphenyl)pyrazole as a white solid. 1H NMR (d6-DMSO) δ: 11.69 (s, 1H), 7.55 (d, 2H), 6.92 (d, 2H), 5.66 (s, 1H), 4.62 (broad s, 2H), 3.75 (s, 3H); HPLC/MS m/z: 190.1 [MH]+.

1. concentrationit was concentrated in vacuo
2. custompurified on silica gel with 0-10% MeOH in CH2Cl2 as eluent