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Hydrochloric Acid → N-[2,2,2-Trifluoro-1-(4-methoxyphenyl)ethylidene]hydroxylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,2,2-Trifluoro-1-(4-phenoxyphenyl)-ethanone oxime | HCID 59115193 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[2,2,2-Trifluoro-1-(4-methoxyphenyl)ethylidene]hydroxylamine | HCID 59115151 | 122.9% |
反応手順
2,2,2-Trifluoro-1-(4-phenoxyphenyl)-ethanone oxime (single isomer) 35 g (124 mmol) of 2,2,2-trifluoro-1-(4-phenoxyphenyl)-ethanone oxime (mixture of E- and Z-isomers) prepared according to the method described in example 80.1 is dissolved in 300 ml of methylene chloride. To the solution is added 1.1 ml of conc. HCl and stirred at room temperature for 4.5 hours. The reaction mixture is washed with water and brine, dried over MgSO4, and concentrated, yielding 33.4 g of 2,2,2-trifluoro-1-(4-methoxyphenyl)-ethanone oxime (single isomer) as a white solid. The structure is confirmed by the 1H-NMR spectrum (CDCl3). δ[ppm]: 7.00-7.12 (m, 4H), 7.19 (t, 1H), 7.39 (t, 2H), 7.57 (d, 2H), 8.95 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06261738B1 |
| 出典データセット | uspto-grants-2001_07 |
| ORD ID | ord-ad3fc87af70f493aa3ad56fb90d74dc7 |
| 出典メモ | uspto-grants-2001_07 |