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Diisopropylethylamine → 4'-Methyl-N-((6-methylpyridin-3-yl)methyl)-5-(methylsulfonyl)biphenyl-3-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 反応物 | (6-Methylpyridin-3-yl)methanamine | HCID 12214337 | — |
| 反応物 | 4'-Methyl-5-(methylsulfonyl)biphenyl-3-carboxylic acid | HCID 58187993 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4'-Methyl-N-((6-methylpyridin-3-yl)methyl)-5-(methylsulfonyl)biphenyl-3-carboxamide | HCID 44223084 | — |
反応手順
To a mixture of 4′-methyl-5-(methylsulfonyl)biphenyl-3-carboxylic acid (40 mg, 0.14 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (53 mg, 0.28 mmol), 1-hydroxybenzotriazole hydrate (21 mg, 0.14 mmol), and CH2Cl2 (3 mL) were added (6-methylpyridin-3-yl)methanamine (25 mg, 0.21 mmol), and N,N-diisopropylethylamine (48 μL, 0.28 mmol). The mixture was stirred at room temperature overnight and then concentrated. The residue was purified by preparative HPLC (100×20.2 mm, C18 column; 30-80% CH3CN-water[10 mM Et2NH]) to afford a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08946439B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-c170afbc6f2b4ca5abc439f359ea46ca |
| 出典メモ | uspto-grants-2015_02 |