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N-bromobutanimide → 1-(Bromomethyl)-2,5-difluoro-4-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 1,4-Difluoro-2-methyl-5-nitrobenzene | HCID 230658 | — |
| 触媒 | Benzoyl Peroxide | HCID 7187 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 1-(Bromomethyl)-2,5-difluoro-4-nitrobenzene | HCID 53403397 | 220.5% |
反応手順
1,4-Difluoro-2-methyl-5-nitrobenzene (1 g) was dissolved in chlorobenzene (6 mL) and N-bromosuccinimide (1.54 g) added followed by benzoyl peroxide (0.2 g). The reaction mixture was stirred at reflux for 2.5 hours then additional benzoyl peroxide (0.2 g) and N-bromosuccinimide (1.54 g) were added. The reaction was refluxed for 2 hours then was cooled to room temperature, quenched with water and extracted with dichloromethane (3×). The combined organics were dried and concentrated under reduced pressure. The oil obtained was triturated with diethyl ether, filtered and the filtrate concentrated under reduced pressure to yield the title compound (3.21 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09108939B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-502793d67fcb49f4b86ae129b0caa852 |
| 出典メモ | uspto-grants-2015_08 |