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Carbon Tetrachloride → 6-Bromomethyl-2-cyclohexyl-benzothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Tetrachloride | HCID 5943 | — |
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 2-Benzyl-6-methyl-benzothiazole | HCID 50849889 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 6-Bromomethyl-2-cyclohexyl-benzothiazole | HCID 57656406 | 53.3% |
反応手順
Combine 2-benzyl-6-methyl-benzothiazole (0.6 g, 2.42 mmol), NBS (0.5 g, 2.54 mmol), AIBN (40 mg, 0.24 mmol), carbon tetrachloride (10 mL) and reflux for 3 h. Cool the reaction mixture to ambient temperature, dilute with chloroform and wash with water. Dry the organic extracts over anhydrous Na2SO4, concentrate in vacuo and purify by chromatography on silica gel eluting with hexane/EtOAc (1:0 and 9:1) to obtain the title compound as a white solid (0.4 g, 53%). MS (ES+) m/z: 311 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08022062B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-bfa01b655c134fa38693c1c683fbef7f |
| 出典メモ | uspto-grants-2011_09 |