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Hydrochloric Acid → 2-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)ethan-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Hydrazinoethanol | HCID 8017 | — |
| 反応物 | Pentanenitrile, 4,4-dimethyl-3-oxo- | HCID 108871 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)ethan-1-ol | HCID 16227877 | 97.3% |
反応手順
A solution of 4,4-dimethyl-3-oxo-pentanenitrile (5.00 g, 40.0 mmol), concentrated HCl (0.1 mL), and 2-hydrazino ethanol (2.98 mL, 44.0 mmol) in ethanol (40 mL) was refluxed for 20 h. The reaction mixture was then concentrated in vacuo. The resulting oily solid was washed with cyclohexane (30 mL), and dissolved in MeOH (5 mL) and H2O (5 mL) and lyophilised to give the title compound as a white powder (7.13 g, 97%). LCMS (Method 3): Rt 0.43 min, m/z 184 [MH+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835431B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-2de6a3d9b2ca4b78bda6fb2329a4e94d |
| 出典メモ | uspto-grants-2014_09 |