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Pyridine → N-(2-Bromophenyl)cinnamamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-Bromoaniline | HCID 11992 | — |
| 反応物 | 3-Phenylprop-2-enoyl chloride | HCID 66023 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-Bromophenyl)cinnamamide | HCID 764332 | 98% |
反応手順
To a mixture of 2-bromobenzenamine (200.0 g, 1163 mmol), pyridine (188.1 ml, 2325 mmol) and dry dichloromethane (1000 ml) at 0° C. was added slowly cinnamoyl chloride (193.7 g, 1163 mmol). The resulting mixture was stirred while warming to ambient temperature overnight. The resulting mixture was washed with sodium bicarbonate (1000 ml), 10% sodium bisulfate (1000 ml), sodium bicarbonate (1000 ml) and brine (1000 ml). The organic layer was dried over MgSO4 and concentrated under reduced pressure to yield title compound as a solid (172.3 gm, 98% yield) MS ESI (+) m/z 224 and 226 (M+1 of each isotope) detected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08138181B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-663da7ac9a59420ba1f1efdc76a512b6 |
| 出典メモ | uspto-grants-2012_03 |