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Pyridine → 4-bromo-N-[(5-bromo-1,3-thiazol-2-yl)carbamoyl]-5-chlorothiophene-2-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Sodium Cyanate | HCID 517096 | — |
| 反応物 | 5-Bromothiazol-2-amine monohydrobromide | HCID 2723848 | — |
| 反応物 | 4-Bromo-5-chlorothiophene-2-sulfonyl chloride | HCID 2797220 | — |
| 触媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-bromo-N-[(5-bromo-1,3-thiazol-2-yl)carbamoyl]-5-chlorothiophene-2-sulfonamide | HCID 24752361 | — |
反応手順
4-Bromo-5-chloro-thiophene-2-sulfonyl chloride (0.44 g, 1.50 mmol) and pyridine (0.27 ml, 3.40 mmol) were added to a stirred suspension of sodium cyanate (0.14 g, 2.20 mmol) in dry acetonitrile (1 ml) and the mixture stirred at room temperature for 4 hours. 5-Bromo-thiazol-2-ylamine hydrobromide (0.26 g, 1.00 mmol) was added and the reaction stirred for 30 minutes. Water (2 ml) and acetic acid (3 drops) were added. The resulting precipitate was filtered and the solid washed with water, cold methanol and diethyl ether. The solid was dried under reduced pressure to give 4-bromo-N-[(5-bromo-1,3-thiazol-2-yl)carbamoyl]-5-chlorothiophene-2-sulfonamide, 0.29 g (60%), m/e 477.8 (MH−).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07868030B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-b7e58246bbc2468bb2c288d11cb2e1de |
| 出典メモ | uspto-grants-2011_01 |