反应详情

EDCI (288 mg, 1.5 mmol) was added to a solution of 1,2-diaminobenzene (0.141 g, 1.31 mmol), 3-phenyl-1H-pyrazole-5-carboxylic acid (188 mg, 1.0 mmol) and HOBT (203 mg, 1.5 mmol) in anhydrous DMF (5 mL). The reaction was stirred under nitrogen at room temperature. After twelve hours the reaction was concentrated in vacuo and precipitated from methanol with a small amount of water. The solid was collected by vacuum filtration and further purified on reverse phase HPLC using water-acetonitrile gradient (0.1% TFA) to provide the corresponding amide (60 mg, 38% yield).

1. concentrationAfter twelve hours the reaction was concentrated in vacuo
2. customprecipitated from methanol with a small amount of water
3. filtrationThe solid was collected by vacuum filtration
4. customfurther purified on reverse phase