関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Methylethylamine | HCID 12219 | — |
| 反応物 | Propylphosphoric anhydride | HCID 16167369 | — |
| 反応物 | HCID 178461212 | HCID 178461212 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178464470 | HCID 178464470 | — |
反応手順
To a reaction vessel was added the crude residue of (S)-1-(4-(5-chloropyridin-3-yl)-6-cyano-3-((trans-4-methylcyclohexyl)methyl)-3H-imidazo[4,5-c]pyridin-2-yl)pyrrolidine-2-carboxylic acid (0.030 g, 0.063 mmol), propylphosphonic anhydride (0.10 mL, 50% w/w in DMF), and N-methylethanamine (0.0037 g, 0.063 mmol) suspended in DMF (0.5 mL). The reaction was stirred at ambient temperature for 6 hours. The reaction was diluted with H2O (2.0 mL) and was extracted with EtOAc (2×5 mL). The combined organics were concentrated in vacuo to afford (S)-1-(4-(5-chloropyridin-3-yl)-6-cyano-3-((trans-4-methylcyclohexyl)methyl)-3H-imidazo[4,5-c]pyridin-2-yl)-N-ethyl-N-methylpyrrolidine-2-carboxamide as a crude residue. MS ESI calc'd. for C28H34ClN7O [M+H]+ 520. found 520.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846657B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-23d6257325894789ba327a40df7272e6 |
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| 出典メモ | uspto-grants-2014_09 |
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