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Triethylamine → HCID 66682491、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Chloropropionitrile | HCID 10963 | — |
| 反応物 | 4-(3-fluoro-4-methoxyphenyl)-N-methyl-N-(piperidin-4-yl)-1H-imidazole-1-carboxamide hydrochloride | HCID 66688407 | — |
| 溶媒 | Isopropanol methylene chloride | HCID 21966342 | — |
| 生成物 | HCID 66682491 | HCID 66682491 | 68% |
反応手順
Triethylamine (0.159 mL, 1.139 mmol) was added to a stirred suspension of 4-(3-fluoro-4-methoxyphenyl)-N-methyl-N-(piperidin-4-yl)-1H-imidazole-1-carboxamide hydrochloride (0.200 g, 0.542 mmol) and 3-chloropropanenitrile (0.058 g, 0.651 mmol) at room temperature. The clear solution was allowed to stir at reflux for 2 h, during which time a white suspension formed. The mixture was allowed to cool to room temperature, diluted with a mixture of dichloromethane/isopropanol (7:3) and then washed with water. The organic layer was dried (MgSO4), filtered and evaporated to give a colourless solid that was triturated with ethanol to give the product (142 mg, 64%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09353082B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-49d03cef0bcb473db520077fc1c788f4 |
| 出典メモ | uspto-grants-2016_05 |