関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Chloro-1-methylpyridinium iodide | HCID 167069 | — |
| 反応物 | (RS)-2-(4-chlorobenzenesulfonylamino)butanoic acid | HCID 3266285 | — |
| 反応物 | Ethyl (4-aminophenyl)acetate--hydrogen chloride (1/1) | HCID 24192282 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | (RS)-2-(4-chlorobenzenesulfonylamino)-N-(4-(ethoxycarbonylmethyl)phenyl)butanamide | HCID 19032983 | 16.7% |
反応手順
Triethylamine (1.99 ml), ethyl 4-aminophenylacetate hydrochloride (699 mg), and 1-methyl-2-chloropyridinium iodide (1.1 g) were added to a solution of (RS)-2-(4-chlorobenzenesulfonylamino)butanoic acid (1 g) in chloroform (30 ml), and the whole was heated under reflux for 2 hours under argon. The reaction mixture was concentrated under reduced pressure. After adding 1N HCl, the residue was extracted with ethyl acetate. The combined ethyl acetate layers were washed with a saturated saline solution, and dried over Na2SO4. The solvent was evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 70 g, hexane/ethyl acetate=2/1) to give (RS)-2-(4-chlorobenzenesulfonylamino)-N-(4-(ethoxycarbonylmethyl) phenyl)butanamide (237 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05650428 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-a74198e9447c4141b53b3f8232f4f299 |
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| 出典メモ | uspto-grants-1997_07 |
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