反应详情

Under argon, 75 mg (039 mmol) of 5-amino-1-cyclopentyl-1H-pyrazole-4-carboxamide and 183 mg (1.16 mmol, 3 equiv.) of methyl cyclohexylacetate are introduced into 1.5 ml of absolute ethanol. At 0° C., 54 mg of sodium hydride (60% dispersion in mineral oil; L35 mmol, 15 equiv.) are slowly added in a countercurrent of argon. The resulting mixture is slowly heated and stirred under reflux for 18 h. For workup, 20 ml of water are added, and the mixture is extracted several times with ethyl acetate. The combined organic phases are dried over sodium sulfate and concentrated in vacuo. The crude product is purified by preparative HPLC.

1. temperatureThe resulting mixture is slowly heated
2. temperatureunder reflux for 18 h
3. extractionthe mixture is extracted several times with ethyl acetate
4. dry with materialThe combined organic phases are dried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe crude product is purified by preparative HPLC