関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Malonic Acid | HCID 867 | — |
| 反応物 | 2,5-Difluoro-4-methoxybenzaldehyde | HCID 3856938 | — |
| 溶媒 | Pyridine ethanol | HCID 21975839 | — |
| 生成物 | (E)-3-(2,5-difluoro-4-methoxy-phenyl)-acrylic acid | HCID 5928340 | 74% |
反応手順
A 250 mL round bottom flask was charged with 2,5-difluoro-4-methyoxybenzaldehyde (commercially available from Manchester Organics Ltd., UK) (18.45 g, 107.2 mmol), malonic acid (commercially available from Sigma-Aldrich, St. Louis, Mo., USA) (12.27 g, 117.9 mmol), and 10:1 EtOH/pyridine (27 mL). The mixture was stirred overnight at 70° C. under a reflux condenser and cooled to 0° C. for 2 hours. The precipitated solid was filtered, rinsed with ether, and dried in vacuo to afford H3.1 (16.96 g, 74% yield) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08748462B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-060b17b6940d4708b390ae4dbd86790d |
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| 出典メモ | uspto-grants-2014_06 |
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