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Azobisisobutyronitrile → 4-(Bromomethyl)-1-chloro-2-methoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 1-Chloro-2-methoxy-4-methylbenzene | HCID 99352 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 4-(Bromomethyl)-1-chloro-2-methoxybenzene | HCID 13662859 | 92% |
反応手順
To a solution of 1-chloro-2-methoxy-4-methyl-benzene (50 g, 0.32 mol) in CCl4 (350 mL) was added NBS (57.2 g, 0.32 mol) and AIBN (10 g, 60 mmol). The mixture was heated at reflux for 3 hours. The solvent was evaporated under vacuum and the residue was purified by column chromatography on silica gel (Petroleum Ether/EtOAc=20:1) to give 4-bromomethyl-1-chloro-2-methoxy-benzene (69 g, 92%). 1H NMR (400 MHz, CDCl3) δ 7.33-7.31 (m, 1H), 6.95-6.91 (m, 2H), 4.46 (s, 2H), 3.92 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741321B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-127a3157d14c402ba00add575389526d |
| 出典メモ | uspto-grants-2010_06 |