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Hydrochloric Acid → 3-tert-butyl-1-(4-(methylsulfonyl)phenyl)-1H-pyrazol-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pentanenitrile, 4,4-dimethyl-3-oxo- | HCID 108871 | — |
| 反応物 | 4-(Methylsulfonyl)phenylhydrazine hydrochloride | HCID 2735181 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 3-tert-butyl-1-(4-(methylsulfonyl)phenyl)-1H-pyrazol-5-amine | HCID 59588828 | — |
反応手順
4-(methylsulfonyl)phenylhydrazine hydrochloride (1.133 g, 5.09 mmol) and 4,4-dimethyl-3-oxopentanenitrile (0.697 g, 5.57 mmol) were weighed into a 100 mL RBF. 0.2 M HCl in EtOH (42 mL) was added and the suspension was heated to reflux for 27 h, during which time all solids gradually dissolved to give a yellow solution. The solution was diluted with 1 M NaOH(aq) (˜16 mL) to pH 12-13, EtOAc (70 mL) was added and the biphasic system was vigorously stirred for 5 min. The organic layer was isolated, dried (MgSO4), filtered and concentrated to give a yellow crystalline solid. Yield: 1.42 g (95%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198279B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-4e01d0d226ac4ac28dcd7f14d33611df |
| 出典メモ | uspto-grants-2012_06 |