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2-Thiophenesulfonyl chloride → N-(4-Bromo-5-methyl-3-isoxazolyl)thiophene-2-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Thiophenesulfonyl chloride | HCID 85518 | — |
| 反応物 | 4-Bromo-5-methyl-1,2-oxazol-3-amine | HCID 2774464 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-(4-Bromo-5-methyl-3-isoxazolyl)thiophene-2-sulfonamide | HCID 22998411 | 51% |
反応手順
Thiophene-2-sulfonyl chloride (183 mg, 1 mmol) was added to a solution of 3-amino-4-bromo-5-methylisoxazole (177 mg, 1 mmol) in dry pyridine (0.5 ml). The reaction mixture was stirred at room temperature for 3 h. Pyridine was removed under reduced pressure and the residue was partitioned between water and ethyl acetate. The organic layer was washed with 1N HCl (3×10 ml), brine (10 ml) and dried over anhydrous magnesium sulfate. Evaporation of the solvents left an oily residue which was solidified at -20° C. and then purified by recrystallization from ethyl acetate/hexanes, to give the pure product (51% yield) as a tan solid, m.p. 156°-158° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05594021 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-98c55c648c034017af90ed529e7f7646 |
| 出典メモ | uspto-grants-1997_01 |