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Diisopropylethylamine → 8-Hydroxy-2-oxo-2H-chromene-3-carboxylic acid [3-(2-ethoxy-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-(2-Ethoxy-pyridin-3-yl)-phenylamine | HCID 66865170 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 8-Hydroxy-2-oxo-2H-chromene-3-carboxylic acid [3-(2-ethoxy-pyridin-3-yl)-phenyl]-amide | HCID 86650369 | 61% |
反応手順
DIEA (0.013 mL, 0.077 mmol) was added to 8-hydroxy-3-carboxy-coumarin (0.014 g, 0.070 mmol) and HATU (0.029 g, 0.077 mmol) in 0.36 mL of DMF with constant stirring at room temperature until a clear solution resulted. Subsequently, 3-(2-Ethoxy-pyridin-3-yl)-phenylamine (0.015 g, 0.070 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 0.017 g of product in 61% yield: LCMS (ESI) m/z 403 (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-0fcad771a3cb4cc98ff296f39c685c90 |
| 出典メモ | uspto-grants-2014_02 |