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Benzoyl Peroxide → 5-(Bromomethyl)-2-chloro-3-fluoropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 2-Chloro-3-fluoro-5-methylpyridine | HCID 13541365 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 5-(Bromomethyl)-2-chloro-3-fluoropyridine | HCID 59297078 | 51% |
反応手順
2-chloro-3-fluoro-5-methylpyridine in an amount of 4.00 g (27.6 mmol) was dissolved in 80 mL of carbon tetrachloride, following which 7.37 g (41.4 mmol) of N-bromosuccinimide and 20 mg of benzoyl peroxide were added and the mixture was refluxed overnight under heating. Following reaction completion, the reaction mixture was returned to room temperature, concentrated under reduced pressure, and purified by silica gel column chromatography (hexane/ethyl acetate=19:1), giving 3.06 g of 5-(bromomethyl)-2-chloro-3-fluoropyridine (yield, 51%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09073866B2 |
| 出典データセット | uspto-grants-2015_07 |
| ORD ID | ord-674710ec3a4f4c3b808d9de8c33f3999 |
| 出典メモ | uspto-grants-2015_07 |