関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1H-1,2,4-Triazole | HCID 9257 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | N-(3-bromo-5-nitrophenyl)acetamide | HCID 10658908 | — |
| 触媒 | HCID 178419072 | HCID 178419072 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(3-nitro-5-(1H-1,2,4-triazol-1-yl)phenyl)acetamide | HCID 117777868 | 86% |
反応手順
To a solution of N-(3-bromo-5-nitrophenyl)acetamide (5 g, 19.3 mmol) in DMF (50 ml) were added 1,2,4-triazole (3.3 g, 48.25 mmol, 2.5 eq.), copper(I) oxide (0.56 g, 3.86 mmol, 0.2 eq.) and cesium carbonate (12.5 g, 38.6 mmol, 2 eq.) and the mixture was heated at 90° C. for 48 h. The mixture was quenched and extracted as in Example 1(d). The solvent was distilled off and the residue was purified by column chromatography (60-120 silica gel, 30% ethyl acetate in hexane) to give the product in 86% yield (4.1 g). LC-MS (ESI): Calculated mass: 247.21; Observed mass: 248.0 [M+H]+ (rt: 0.257 min).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09447091B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-a13152e7742742738e129b0fe1ef8d0a |
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| 出典メモ | uspto-grants-2016_09 |
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