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Ethyl Bromide → HCID 178436371、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Bromide | HCID 6332 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | [(3-Ethylphenyl)amino]carbonitrile | HCID 10012043 | — |
| 反応物 | N-(m-ethylphenyl)-N-ethylcyanamide | HCID 10442201 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178436371 | HCID 178436371 | 88% |
反応手順
N-(m-Ethylphenyl)-N-ethylcyanamide: A suspension of m-ethylphenylcyanamide (2.26 g, 15.45 mmol) and sodium hydride (820 mg, 34.2 mmol, pre-washed thrice with hexane) in anhydrous THF (20 ml) was heated at 80°-85° C. for 2.5 hours. After it was allowed to cool to room temperature ethyl bromide (4.66 g, 42.76 mmol) was added and continued stirring at room temperature for 6 hours. Methanol (20 ml) followed by water (40 ml) were added and then extracted with dichloromethane (3×25 ml). Concentration of the organic layer followed by quick flash chromatography afforded the title compound (2.36 mg, 88%) as a light yellow liquid:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05767162 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-3ec3ad3d56a3403b9c70b3acc494d195 |
| 出典メモ | uspto-grants-1998_06 |