関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 5-Chloro-2-methoxy-4-methylpyridine | HCID 23133646 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Bromo-5-chloro-2-methoxy-4-methylpyridine | HCID 23133645 | 97.4% |
反応手順
20.2 g (114 mmol) of N-bromosuccinimide was charged to a N,N-dimethylformamide (DMF) 15 ml solution of 7.2 g (46 mmol) of 5-chloro-2-methoxy-4-methylpyridine, followed by stirring at 50° C. for 20 hours. A diluted sodium thiosulfate aqueous solution was added to the reaction solution, and the aqueous layer was extracted with diethyl ether. The organic layer was washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate and subjected to filtration on the pad of a silica gel cake, and the solvent was distilled off under reduced pressure to obtain 10.6 g (yield: 97%) of 3-bromo-5-chloro-2-methoxy-4-methylpyridine (melting point: 44 to 45° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08653113B2 |
|---|
| 出典データセット | uspto-grants-2014_02 |
|---|
| ORD ID | ord-8ad5921db5894f448d59391ae3c2d45b |
|---|
| 出典メモ | uspto-grants-2014_02 |
|---|