反应详情

A suspension of 3-(3-methylquinoxalin-2-yl)-3-oxopropanenitrile (45.8 g, 217 mmol) and hydrazine monohydrate (15.8 mL, 325 mmol) in acetic acid (109 mL) and ethanol (1083 mL) was refluxed for 17 h. After being cooled to ambient temperature, the reaction mixture was diluted with water (360 mL) and basified to pH 8 with sodium bicarbonate. The resulting precipitate was collected and washed with diisopropyl ether. The crude was diluted with methanol (1077 mL) and potassium carbonate (29.9 g), and then heated at 60° C. for 2 h. The precipitate was collected and washed with diisopropyl ether to give 3-(3-methylquinoxalin-2-yl)-1H-pyrazol-5-amine. MS (APCI): m/z 226 (M+H).

1. temperaturewas refluxed for 17 h
2. customThe resulting precipitate was collected
3. washwashed with diisopropyl ether
4. additionThe crude was diluted with methanol (1077 mL) and potassium carbonate (29.9 g)
5. temperatureheated at 60° C. for 2 h
6. customThe precipitate was collected
7. washwashed with diisopropyl ether