関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 1-(2-(6-(6-amino-pyridin-3-yloxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-1-yl)-ethanone | HCID 23145367 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 131728153 | HCID 131728153 | — |
反応手順
0.003 ml of ethyl chloroformate was added to a pyridine (1 ml) solution of 14.4 mg of 1-(2-(6-(6-amino-pyridin-3-yloxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-1-yl)-ethanone obtained in Example 340 (step 1), and the reaction liquid was stirred at room temperature for 30 minutes. The reaction liquid was distilled under reduced pressure, and the resulting residue was dissolved in 1 ml of trifluoroacetic acid, and the reaction liquid was stirred at room temperature for 1 hour. The reaction liquid was distilled under reduced pressure, and the resulting residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid] and through silica gel column chromatography (developing solvent: chloroform/methanol=9/1) to obtain the entitled compound as a yellow oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728025B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-2a0180ebe4b145b8a883237ce4e9197a |
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| 出典メモ | uspto-grants-2010_06 |
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