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Hydrochloric Acid → 3-Amino-1-phenyl-1H-pyrazole-4-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Propanedinitrile, [[(4-cyano-1-phenyl-1H-pyrazol-3-yl)amino]methylene]- | HCID 8005203 | — |
| 生成物 | 3-Amino-1-phenyl-1H-pyrazole-4-carbonitrile | HCID 2774249 | — |
| 生成物 | 3-amino-1-phenyl-1H-pyrazole-4-carboxamide | HCID 8831909 | — |
反応手順
{[(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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08415346B2 |
| 出典データセット | uspto-grants-2013_04 |
| ORD ID | ord-005bf0f697e94a12a37f452a8ace5874 |
| 出典メモ | uspto-grants-2013_04 |