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Diisopropylethylamine → (S)-N3-(2-Hydroxy-1-(6-methoxypyridin-3-yl)ethyl)-N5-isobutyl-N5,4'-dimethylbiphenyl-3,5-dicarboxamide
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 | (S)-2-Amino-2-(6-methoxypyridin-3-yl)ethanol | HCID 55278315 | — |
| 反応物 | 5-(Isobutyl(methyl)carbamoyl)-4'-methylbiphenyl-3-carboxylic acid | HCID 58188089 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (S)-N3-(2-Hydroxy-1-(6-methoxypyridin-3-yl)ethyl)-N5-isobutyl-N5,4'-dimethylbiphenyl-3,5-dicarboxamide | HCID 58188092 | — |
反応手順
To a mixture of 5-(isobutyl(methyl)carbamoyl)-4′-methylbiphenyl-3-carboxylic acid (35 mg, 0.11 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (41 mg, 0.22 mmol), 1-hydroxybenzotriazole hydrate (16 mg, 0.11 mmol), CH2Cl2 (3 mL) were added (S)-2-amino-2-(6-methoxypyridin-3-yl)ethanol (27 mg, 0.16 mmol) (WO 2008/130481) and N,N-diisopropylethylamine (28 pt, 0.16 mmol). The mixture was stirred at room temperature overnight, and then concentrated in vacuo. The residue was purified by preparative HPLC (100×21.2 mm C18 column, 30-70% MeCN/water[10 mM Et2NH]) to yield 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-91bab574a0cd475e924e133f01be886e |
| 出典メモ | uspto-grants-2015_02 |