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4-Phenylbenzoyl chloride → N-(5-Chloropyridin-2-yl)-2-(4-phenylbenzoylamino)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Phenylbenzoyl chloride | HCID 84151 | — |
| 反応物 | 2-amino-N-(5-chloropyridin-2-yl)benzamide | HCID 21906381 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(5-Chloropyridin-2-yl)-2-(4-phenylbenzoylamino)benzamide | HCID 21906587 | 94% |
反応手順
To a solution of N-(5-chloropyridin-2-yl)-2-aminobenzamide (0.247 g, 1 mmol) in dichloromethane (10 mL) and pyridine (0.5 mL) was added a solution of 4-biphenylcarbonyl chloride (0.217 g, 1 mmol) in dichloromethane (5 mL). After stirring overnight the solvent was removed in vacuo. The residue was partitioned between ethyl acetate (50 mL) and water (25 mL). Separate the layers and wash the organic layer with water (2×10 mL), saturated sodium bicarbonate (2×20 mL), hydrochloric acid (0.2 N, 1×20 mL). Dried over MgSO4, filtered and concentrated in vacuo. The residue was then purified by RPHPLC (30% ethyl acetate/hexane) to give 0.4 g (94%) of pure product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129245B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-198ee1f97c8c47cdb4df893751253757 |
| 出典メモ | uspto-grants-2006_10 |