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Ethanol → (p-Chlorophenyl)-1,1,1-trifluoro-2-propanone oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 3-(4-Chlorophenyl)-1,1,1-trifluoropropan-2-one | HCID 15113983 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (p-Chlorophenyl)-1,1,1-trifluoro-2-propanone oxime | HCID 85405208 | 110.7% |
反応手順
A solution of 3-(p-Chlorophenyl)-1,1,1-trifluoro-2-propanone (10.0 g, 0.045 mol) and ethanol (60 mL) is treated with a solution of hydroxylamine hydrochloride (4.68 g, 0.067 mol) and water (20 mL) and then with a solution of sodium acetate (5.53 g, 0.067 mol) and water (20 mL). The reaction mixture is then refluxed for 2 hours, cooled to room temperature, diluted with water and extracted with ether. The combined organic extracts are washed sequentially with water and brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give a liquid which solidifies upon standing to give the title product as white needles (11.84 g). Identified by IR and NMR spectral analyses.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05229524 |
| 出典データセット | uspto-grants-1993_07 |
| ORD ID | ord-b262fd9b53444af0a49d60b931edfa21 |
| 出典メモ | uspto-grants-1993_07 |