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乙腈 → 5-chloro-2,4-difluoro-N-pyridazin-3-ylbenzenesulfonamide
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 乙腈 | HCID 6342 | — |
| 反应物 | 三乙烯二胺 | HCID 9237 | — |
| 反应物 | 3-氨基哒嗪 | HCID 230373 | — |
| 反应物 | 5-氯-2,4-二氟苯磺酰氯 | HCID 2773527 | — |
| 产物 | 5-chloro-2,4-difluoro-N-pyridazin-3-ylbenzenesulfonamide | HCID 59436556 | 24.9% |
反应步骤
Pyridazin-3-amine (1.00 g, 10.5 mmol) and triethylenediamine (1.18 g, 10.5 mmol) was added concurrently to a solution of 5-chloro-2,4-difluorobenzenesulfonyl chloride (2.60 g, 10.5 mmol) in acetonitrile (50 mL, 1000 mmol). The reaction mixture was stirred for 18 h then concentrated. The residue was dissolved in ethyl acetate (30 mL), washed with water, brine, dried over sodium sulfate and concentrated. The residue was purified on automated silica gel chromatography (chloroform to 50% of 10% methanol in chloroform) to give 800 mg of the desired product as a yellow solid.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US08541588B2 |
| 来源数据集 | uspto-grants-2013_09 |
| ORD ID | ord-69c130f46a43405c8ab272fa1855e7ad |
| 来源说明 | uspto-grants-2013_09 |