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Acetic Acid → 4-{[(5-Chloro-6-isopropoxypyridin-3-yl)oxy]methyl}-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Chloro-6-isopropoxypyridin-3-OL | HCID 58042436 | — |
| 反応物 | 4-(Bromomethyl)-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide | HCID 89619586 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-{[(5-Chloro-6-isopropoxypyridin-3-yl)oxy]methyl}-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide | HCID 71616019 | 30% |
反応手順
A solution of 5-chloro-6-isopropoxypyridin-3-ol (Preparation 6, 44 mg, 0.232 mmol), 4-(bromomethyl)-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide (Preparation 1, 83 mg, 0.23 mmol) and potassium carbonate (64 mg, 0.47 mmol) in dimethyl sulfoxide (5 mL) was stirred at room temperature for 16 hours. The reaction mixture was diluted with water (20 mL) and acidified to ˜pH 4 using acetic acid (2 mL). The resulting precipitate was filtered, washed with water (20 mL) and dried to afford the title compound as a white solid (32 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09085517B2 |
| 出典データセット | uspto-grants-2015_07 |
| ORD ID | ord-a284f27bbef3449894fcd3114f1fa3f0 |
| 出典メモ | uspto-grants-2015_07 |