化工社化工社 化学情報印刷レポート · 研究参考用
Chlorosuccinimide → 3-fluoro-N-hydroxybenzene-1-carbonimidoyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | (E)-N-[(3-Fluorophenyl)methylidene]hydroxylamine | HCID 5582750 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-fluoro-N-hydroxybenzene-1-carbonimidoyl chloride | HCID 14221338 | 73% |
反応手順
To a solution of (E)- and/or (Z)-3-fluoro-benzaldehyde oxime (6.9 g, 50 mmol) in DMF (50 mL) was added N-chlorosuccinimide (6.6 g, 50 mmol) portionwise over 1 h, keeping the temperature below 35° C. The reaction mixture was stirred at room temperature for 1 h. The mixture was then poured onto ice-water, and extracted with ethyl acetate. The combined organic layers were then washed with water and brine, dried over sodium sulfate and evaporated to afford the title compound (6.3 g, 73%) which was obtained as an off white solid. MS m/e (EI): 173.1 [M].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846719B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-91e8c48a772f4e2392986e130f39e660 |
| 出典メモ | uspto-grants-2014_09 |