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Diisopropylethylamine → 8-Hydroxy-2-oxo-2H-chromene-3-carboxylic acid [3-(5-methoxy-pyridin-3-yl)-phenyl]-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 8-Hydroxy-3-carboxy-coumarin | HCID 7245716 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 反応物 | 3-(5-Methoxy-pyridin-3-yl)-phenylamine | HCID 66865720 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 8-Hydroxy-2-oxo-2H-chromene-3-carboxylic acid [3-(5-methoxy-pyridin-3-yl)-phenyl]-amide | HCID 86650427 | 56% |
反応手順
DIEA (0.012 mL, 0.071 mmol) was added to 8-hydroxy-3-carboxy-coumarin (0.013 g, 0.065 mmol) and HATU (0.027 g, 0.071 mmol) in 0.5 mL of DMF with constant stirring at room temperature until a clear solution resulted. Subsequently, 3-(5-methoxy-pyridin-3-yl)-phenylamine (0.013 g, 0.065 mmol) was added and allowed to react overnight when a solid precipitated out of solution. The resulting precipitate was filtered, dried under suction, and finally dried overnight in vacuo to give 0.014 g of product in 56% yield: LCMS (ESI) m/z 389 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08642788B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-4f2bad91458344408400b0ffb5e83ce0 |
| 出典メモ | uspto-grants-2014_02 |