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Ethyl Acetate → 5-Amino-1-(1-naphthyl)-3-(4-tolyl)pyrazole-4-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Hydrazine, 1-naphthalenyl-, hydrochloride (1:1) | HCID 519949 | — |
| 反応物 | 2-Cyano-3-methylthio-3-(4-tolyl)acrylamide | HCID 54242237 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 5-Amino-1-(1-naphthyl)-3-(4-tolyl)pyrazole-4-carboxamide | HCID 54355348 | 27% |
反応手順
The title compound was prepared from 2-cyano-3-methylthio-3-(4-tolyl) acrylamide (464 mg, 2.0 mmol), 1-naphthyl hydrazine hydrochloride (389 mg, 2.0 mmol) and sodium hydroxide (88 mg, 2.2 mmol) following the procedure used for the compound of Example 12. The crude product was subjected to column chromatography (SiO2, 50-60% ethyl acetate in hexane) and was recrystallised from diethylether to give the title compound as pink crystals (185 mg) m.p. 195°. δH (CDCl3) 8.00 (1H, d, J 8.3 Hz), 7.95 (1 H., m), 7.73-7.55 (7H, m), 7.30 (2H, d, J 8.3 Hz), 5.52 (2H, br s), 5.16 (2H, br s) and 2.42 (3H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05922741 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-ef930def809749ab9ca3e9e30e78bcdb |
| 出典メモ | uspto-grants-1999_07 |