関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Fluorobenzoyl chloride | HCID 9808 | — |
| 反応物 | 2-Aminothiophene-3-carboxamide | HCID 699495 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-(2-Fluorobenzamido)thiophene-3-carboxamide | HCID 7164102 | 77% |
反応手順
2-Amino-thiophene-3-carboxylic acid amide (8.73 g, 61.4 mmole) was dissolved in pyridine (100 ml), cooled to 0° C., and 2-fluorobenzoyl chloride was added dropwise over 20 min, then the reaction was allowed to warm to room temperature with stirring overnight. The pyridine was removed under vacuum, dichloromethane and water were added. The product was precipitated as a grey solid and was washed with diluted hydrochloric acid, water and air dried. The dichloromethane layer was separated, washed with diluted hydrochloric acid, and water, dried over sodium sulfate (anh.) and the solvent was removed to give a total of 12.45 g product (77% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07977342B2 |
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| 出典データセット | uspto-grants-2011_07 |
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| ORD ID | ord-863d6cffb27e476494e14d237ff3589b |
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| 出典メモ | uspto-grants-2011_07 |
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