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N-bromobutanimide → 1-(Bromomethyl)-4-chloro-2-iodobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Benzene, 4-chloro-2-iodo-1-methyl- | HCID 141766 | — |
| 触媒 | Benzoyl Peroxide | HCID 7187 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 1-(Bromomethyl)-4-chloro-2-iodobenzene | HCID 12930961 | 64.6% |
反応手順
A mixture of 4-chloro-2-iodo-1-methylbenzene (3.95 g, 15.6 mmol), N-bromosuccinimide (3.10 g, 17.6 mmol), and benzoyl peroxide (0.1 g) in carbon tetrachloride (100 mL) was heated to reflux for 48 hours, filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 4:100 ethyl acetate/hexanes to provide 3.34 g (64%) of the desired product. MS (DCI/NH3) m/z 330, 332 (M+H)30; 1H NMR (CDCl3) δ 7.85 (d, 1H), 7.40-7.32 (m, 2H), 4.59 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07211595B2 |
| 出典データセット | uspto-grants-2007_05 |
| ORD ID | ord-0c73544aaf074639b176ee31bd481435 |
| 出典メモ | uspto-grants-2007_05 |