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Hydroxylamine HCl → 2,2,2-Trifluoro-1-p-tolyl-ethanone oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxylamine HCl | HCID 21645 | — |
| 反応物 | 4-(Trifluoroacetyl)toluene | HCID 136237 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,2,2-Trifluoro-1-p-tolyl-ethanone oxime | HCID 57353441 | 73.4% |
反応手順
49.5 g (0.263 mol) of 2,2,2-trifluoro-1-(4-methylphenyl)-ethanone are dissolved in 250 ml of ethanol at 80° C. To the solution are added dropwise 19.2 g (0.276 mol) of hydroxylammonium chloride and 36.7 g (0.447 mol) of sodium acetate dissolved in 125 ml of water. The reaction mixture is refluxed for 3.5 hours. The mixture is poured into ice water, affording a white solid. The filtration yields 39.2 g of 2,2,2-trifluoro-1-(4-methylphenyl)-ethanone oxime as a white solid, mp. 54-68° C. The crude product is used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06512020B1 |
| 出典データセット | uspto-grants-2003_01 |
| ORD ID | ord-ecf269ff19ff4f64b84ccb3d7bd6fb1c |
| 出典メモ | uspto-grants-2003_01 |