関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propionic anhydride | HCID 31263 | — |
| 反応物 | 4-Fluorobenzaldehyde | HCID 68023 | — |
| 反応物 | Sodium Propionate | HCID 2723816 | — |
| 生成物 | CID 367964 | HCID 367964 | — |
反応手順
p-Fluorobenzaldehyde (200 g, 1.61 mol), propionic anhydride (3.5 g, 2.42 mol) and sodium propionate (155 g, 1.61 mol) are mixed in a one liter three-necked flask which had been flushed with nitrogen. The flask is heated gradually in an oil-bath to 140° C. After 20 hours, the flask is cooled to 100° C. and poured into 8 l of water. The precipitate is dissolved by adding potassium hydroxide (302 g) in 2 l of water. The aqueous solution is extracted with ether, and the ether extracts are washed with potassium hydroxide solution. The combined aqueous layers are filtered, are acidified with concentrated HCl, and are filtered. The collected solid, p-fluoro-α-methylcinnamic acid, is washed with water, and is dried and used as obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06699894B1 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-6efc3b3c28c54bd1a91d9c35dff01a04 |
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| 出典メモ | uspto-grants-2004_03 |
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