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Dimethylformamide → (2-(Pyrid-4-yl)-1H-benzimidazole-4-carbonyl)-(L)-valinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733286 | — |
| 反応物 | 2-Pyridin-4-yl-3H-benzoimidazole-4-carboxylic acid | HCID 11207170 | — |
| 生成物 | (2-(Pyrid-4-yl)-1H-benzimidazole-4-carbonyl)-(L)-valinamide | HCID 11416447 | — |
反応手順
120 mg (0.5 mmol) of 2-(pyrid-4-yl)-1H-benzimidazole-4-carboxylic acid (1d) and 76.4 mg (0.5 mmol) of H-(L)-valinamide were dissolved in 5 ml of DMF. 164 mg (0.5 mmol) of TOTU and 0.086 ml of diisopropylethylamine were added and the mixture was stirred at RT for 3 h. The precipitate was filtered off and the filtrate was concentrated. The residue was dissolved in ethyl acetate, the solution was washed with saturated sodium chloride solution, and the organic phase was dried using anhydride sodium sulfate and concentrated. Yield: 168 mg (99%). (M+H)+=338.2 (Cl+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06358978B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-cc209c226de84ecb942c3b52c5f48169 |
| 出典メモ | uspto-grants-2002_03 |