関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Phenylhydrazine | HCID 7516 | — |
| 反応物 | Ethyl 4,4,4-trifluoroacetoacetate | HCID 67793 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178516151 | HCID 178516151 | 98% |
反応手順
18.4 g (0.1 mole) of ethyl 4,4,4-trifluoroacetoacetate was dissolved in 12.0 g (0.2 mole) of acetic acid. The solution was cooled to 10° C. or lower with stirring. Thereto was dropwise added, in 0.5 hour, 11.8 g (0.11 mole) of phenylhydrazine. After the dropwise addition, the mixture was stirred at room temperature for 1 hour and successively at 80° C. for 5 hours to give rise to a reaction. After the reaction, the mixture was cooled to room temperature. Thereto were added 100 ml of water. The resulting crystals were collected by filtration, washed with 50 ml of water twice, and dried in a hot-air drier, to obtain 22.3 g (yield: 98.0%) of a title compound as light yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07812175B2 |
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| 出典データセット | uspto-grants-2010_10 |
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| ORD ID | ord-ccef4bbee4aa4a869de99b8b2947ce1a |
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| 出典メモ | uspto-grants-2010_10 |
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