関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Chloroaniline | HCID 7812 | — |
| 反応物 | Butanoic acid, 4-chloro-3-oxo- | HCID 119720 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Chloropyruvaldehyde 4-chlorophenylhydrazone | HCID 88676367 | 97% |
反応手順
In a mixture of 500 ml of water and 250 ml of concentrated hydrochloric acid is dissolved 128 g of p-chloroaniline. To this solution is added dropwise a solution of 69 g of sodium nitrite in 100 ml of water, while the reaction temperature is maintained at 0° C. Then, to the reaction mixture is added a solution of 136.5 g of 4-chloroacetoacetic acid in 200 ml of water, while the reaction temperature is maintained within the range from 0° C. to 5° C., followed by further addition of a solution of 164 g of sodium acetate in 300 ml of water, whereupon yellow precipitate is produced while bubbling vigorously. The reaction mixture is stirred at a room temperature until the bubbling ceases, followed by collecting the crystals by filtration, washing with water and drying, whereby 224 g of the subject compound is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04621144 |
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| 出典データセット | uspto-grants-1986_11 |
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| ORD ID | ord-1ffff2bd00264ab29292faecc340d5a2 |
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| 出典メモ | uspto-grants-1986_11 |
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