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Ammonium Chloride → 1H-Indole-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Indole-2-carboxylic acid | HCID 72899 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 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 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1H-Indole-2-carboxamide | HCID 594832 | — |
反応手順
To a solution of indole-2-carboxylic acid (1e: 1 mmol) in DMF (4 mL) was added DIPEA (2 eq.) followed by HATU (1.2 eq.). The mixture was stirred for 15 minutes before the desired amine (R6—NH2) was added. The mixture was left to stir at room temperature for 5-16 hrs before saturated NH4Cl solution was added. The mixture was extracted with ethyl acetate and the combined organic extracts were washed with water and brine, dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The crude material was purified on CombiFlash® purification system (Teledyne Isco) using appropriate mixtures of ethyl acetate and cyclohexanes to obtain the desired product indole-2-carboxamide (I).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447039B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-3464dd8d004140eca2db07302f7e781e |
| 出典メモ | uspto-grants-2016_09 |