反应详情

{[(4-cyano-1-phenyl-1H-pyrazol-3-yl)amino]methylene}malononitrile (1.07 g, 4.11 mmol) was stirred in refluxing dioxane (80 mL)/2 N HCl (80 mL) for 3 days. Room temperature was attained and the products extracted into EtOAc (×2). The combined organic extracts were washed with brine, dried over MgSO4 and concentrated in vacuo. Purification of the residue by MPLC (12-100% EtOAc-hexanes followed by 0-10% MeOH-EtOAc) gave 3-amino-1-phenyl-1H-pyrazole-4-carbonitrile as a beige solid (A) and 3-amino-1-phenyl-1H-pyrazole-4-carboxamide as a brown solid (B).

1. customRoom temperature
2. extractionthe products extracted into EtOAc (×2)
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customPurification of the residue by MPLC (12-100% EtOAc-hexanes followed by 0-10% MeOH-EtOAc)