関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Methylphenylhydrazine monohydrochloride | HCID 12504 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Isopropyl Acetate | HCID 7915 | — |
| 生成物 | Acetic acid, 2-(4-methylphenyl)hydrazide | HCID 539992 | — |
反応手順
104.8 g of 1-(4-methylphenyl)hydrazine hydrochloride are suspended in 525 ml of isopropyl acetate, a solution of 104.8 g of potassium carbonate in 300 ml of water is added and then the mixture is stirred until the solid has disappeared. 77.4 g of acetic anhydride are added while maintaining the temperature below 20° C. and then the mixture is left stirring at 20° C. A precipitate is observed to form, which precipitate disappears when the mixture is heated at approximately 55-60° C. The organic phase is washed twice with 200 ml of water and is then cooled at 0-5° C. overnight. The product formed is recovered by filtration and is then washed twice with 100 ml of MTBE.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07816368B2 |
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| 出典データセット | uspto-grants-2010_10 |
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| ORD ID | ord-098942d3eec742f79f27af9508a2a296 |
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| 出典メモ | uspto-grants-2010_10 |
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