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2,4-Difluorobenzenesulfonyl Chloride → N-(5-bromo-2-methoxypyridin-3-yl)-2,4-difluorobenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4-Difluorobenzenesulfonyl Chloride | HCID 2734273 | — |
| 反応物 | 5-Bromo-2-methoxypyridin-3-amine | HCID 44754869 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-(5-bromo-2-methoxypyridin-3-yl)-2,4-difluorobenzenesulfonamide | HCID 59859951 | 31.7% |
反応手順
To a cooled (0° C.) solution of 5-bromo-2-(methyloxy)-3-pyridinamine (20.3 g, 100 mmol) in pyridine (200 mL) was added slowly 2,4-difluorobenzenesulfonyl chloride (21.3 g, 100 mmol) over 15 min (reaction became heterogeneous). The ice bath was removed and the reaction was stirred at ambient temperature for 16 h, at which time the reaction was diluted with water (500 mL) and the solids filtered off and washed with copious amounts of water. The precipitate was dried in a vacuum oven at 50° C. to give N-[5-bromo-2-(methyloxy)-3-pyridinyl]-2,4-difluorobenzenesulfonamide (12 g, 31.6 mmol, 31.7% yield) MS (ES)+ m/e 379.0, 380.9 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08633187B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-7567aa01bda94c738c78c4bf8ce7f168 |
| 出典メモ | uspto-grants-2014_01 |