関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 6-Phenylnicotinic acid | HCID 120118 | — |
| 反応物 | Tert-butyl 3-amino-[1,1'-biphenyl]-4-carboxylate | HCID 58508425 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Tert-butyl 4-phenyl-2-(6-phenylpyridine-3-carboxamido)benzoate | HCID 58508784 | — |
反応手順
N,N-Dimethylformamide (0.9 μl) and oxalyl chloride (0.023 mL) were added to a methylene chloride (0.5 mL) suspension of 6-phenylpyridine-3-carboxylic acid (44 mg) at room temperature, followed by stirring at the same temperature for 1 hour. The reaction mixture was added to a solution mixture of tert-butyl 2-amino-4-phenylbenzoate (40 mg) in methylene chloride (1 mL) and triethylamine (0.17 mL) at room temperature, followed by stirring at same temperature for 1 hour. The solvent was evaporated under reduced pressure, and ethyl acetate and a 10% aqueous solution of citric acid were added to the residue. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [Trikonex AB, FlashTube 2008, eluent: hexane/ethyl acetate=2:1] to obtain tert-butyl 4-phenyl-2-(6-phenylpyridine-3-carboxamido)benzoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08492582B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-b23b938d89394061a5e26b7d882a9d40 |
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| 出典メモ | uspto-grants-2013_07 |
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