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Dichloromethane → N-[3-[(Z)-N'-hydroxycarbamimidoyl]thiophen-2-yl]-2-(4-methoxyphenyl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | N-(3-cyanothiophen-2-yl)-2-(4-methoxyphenyl)acetamide | HCID 2404093 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | N-[3-[(Z)-N'-hydroxycarbamimidoyl]thiophen-2-yl]-2-(4-methoxyphenyl)acetamide | HCID 178490500 | — |
反応手順
To a solution of N-(3-cyanothiophen-2-yl)-2-(4-methoxyphenyl)acetamide (234 mg, 0.859 mmol) in a mixture of ethanol (5 mL), methylene chloride (0.5 mL) and triethylamine (202 4, 1.46 mmol) was added hydroxylamine hydrochloride (90 mg, 1.29 mmol). The resulting solution was stirred at room temperature for 18 h and was subsequently diluted with saturated aqueous sodium bicarbonate and extracted with ethyl acetate. The organic phases were combined, dried (Na2SO4), filtered, concentrated under vacuum and purified on a silica gel column (eluant hexane/ethyl acetate, 7/3 to 2/8) to give N-(3-(N-hydroxycarbamimidoyl)thiophen-2-yl)-2-(4-methoxyphenyl)acetamide. Retention time (min)=1.161, method [1], MS (ESI) 306.1 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08450363B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-8e82bdd650154a31b565d65e00c8be17 |
| 出典メモ | uspto-grants-2013_05 |