HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → 5-chloro-2,4-difluoro-N-pyridazin-3-ylbenzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Dabco | HCID 9237 | — |
| Reactant | Aminopyridazine | HCID 230373 | — |
| Reactant | 5-Chloro-2,4-difluorobenzenesulphonyl chloride | HCID 2773527 | — |
| Product | 5-chloro-2,4-difluoro-N-pyridazin-3-ylbenzenesulfonamide | HCID 59436556 | 24.9% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08153814B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-1832696f37b2473485aafc3f1057d48d |
| Source note | uspto-grants-2012_04 |