HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 178513311, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 4-chloro-N-(4-cyano-benzyl)-N-(2-oxo-azepan-3-yl)-benzenesulfonamide | HCID 18455143 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178513311 | HCID 178513311 | 77.2% |
Reaction Steps
4-Chloro-N-(4-cyano-benzyl)-N-(2-oxo-azepan-3-yl)-benzenesulfonamide (2.09 g, 5.00 mmol), sodium bicarbonate (0.52 g, 6.15 mmol) and hydroxylamine hydrochloride (0.43 g, 6.15 mmol) in a mixture of 20 ml ethanol and 4 ml water were refluxed for 11 hours. The solvents were removed by distillation and the residue was recrystalized from water. The solid was then suspended in dichloromethane, refluxed, cooled to room temperature and filtered to yield 1.74 g (77%) 4-{[(4-chloro-benzenesulfonyl)-(2-oxo-azepan-3-yl)-amino]-methyl}-N-hydroxy-benzamidine as white solid, MS: m/e (%)=451.0 (MH+, 100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07253158B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-3c806657716a47f083890e597ced3c06 |
| Source note | uspto-grants-2007_08 |