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3-Cyanobenzoic acid → 3-cyano-N-(3-ethyl-1-phenyl-1H-indazol-6-yl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Cyanobenzoic acid | HCID 15875 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 3-ethyl-1-phenyl-1H-indazol-6-amine hydrochloride | HCID 67449229 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-cyano-N-(3-ethyl-1-phenyl-1H-indazol-6-yl)benzamide | HCID 58483606 | — |
反応手順
Into a 100-mL round-bottom flask, was placed a solution of 3-ethyl-1-phenyl-1H-indazol-6-amine hydrochloride (1 g, 3.60 mmol, 1.00 equiv, 98%) in dichloromethane (50 mL), 3-cyanobenzoic acid (646.8 mg, 4.31 mmol, 1.20 equiv), TEA (445 mg, 4.31 mmol, 1.20 equiv), EDCI (845 mg, 4.31 mmol, 1.20 equiv). The resulting solution was stirred for 5 h at room temperature. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:3). The collected fractions were combined and concentrated under vacuum to yield 3-cyano-N-(3-ethyl-1-phenyl-1H-indazol-6-yl)benzamide as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822447B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-c9885fe5911146dc96984cf3bded2107 |
| 出典メモ | uspto-grants-2014_09 |