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Acetonitrile → 5-chloro-2,4-difluoro-N-pyridazin-3-ylbenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | Aminopyridazine | HCID 230373 | — |
| 反応物 | 5-Chloro-2,4-difluorobenzenesulphonyl chloride | HCID 2773527 | — |
| 生成物 | 5-chloro-2,4-difluoro-N-pyridazin-3-ylbenzenesulfonamide | HCID 59436556 | 24.9% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541588B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-69c130f46a43405c8ab272fa1855e7ad |
| 出典メモ | uspto-grants-2013_09 |