HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloride 2-chloropyridinium 1-oxide → HCID 22118704, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloride 2-chloropyridinium 1-oxide | HCID 88478 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | N-Boc-N-methylethylenediamine | HCID 2756424 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | 2-Methyl-2-butanol | HCID 6405 | — |
| Product | HCID 22118704 | HCID 22118704 | — |
Reaction Steps
A mixture of N-Boc-N-(methyl)ethylenediamine (Synth. Commun. 1993, 23, 2443-2449)(849.2 mg, 4.87 mmol), 2-chloropyridine N-oxide hydrochloride (970 mg, 5.84 mmol), and NaHCO3 (2.05 g, 24.4 mmol) in tert-amyl alcohol (12 mL) was heated at reflux under argon. After 41.5 h, the reaction was cooled, diluted with EtOH, filtered, and concentrated. The residue was reconcentrated from toluene and chromatographed (silica gel, 5% CH3OH/CHCl3) to give the title compound as a viscous, yellow oil which was used without further purification (863.1 mg, 66%), MS (ES) m/e 268 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06159964 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-1e413e5995a74e699800086e8519890d |
| Source note | uspto-grants-2000_12 |