HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-(3-Chloropyrid-2-ylmethylthio)ethylamine → N,N'-bis-[2-(3-chloropyrid-2-ylmethylthio)ethyl]amidinosulphonic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-(3-Chloropyrid-2-ylmethylthio)ethylamine | HCID 12951532 | — |
| Reactant | 1-Methylthio-1-methyliminomethanesulphonate | HCID 86737078 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | N,N'-bis-[2-(3-chloropyrid-2-ylmethylthio)ethyl]amidinosulphonic acid | HCID 53709668 | — |
Reaction Steps
A solution of 2-(3-chloropyrid-2 ylmethylthio)ethylamine (4.06 g) in dry acetonitrile (200 ml) was added dropwise, with stirring, to a solution of 1-methylthio-1-methyliminomethanesulphonate (1.69 g) in dry acetonitrile (150 ml) at 50°. The mixture was stired at 60° for 1 hour and then allowed to cool. The mixture was evaporated to dryness, dissolved in methanol and absorbed onto silica gel. Chromatography on a column of silica gel produced a viscous oil which was collected by eluting the column with a chloroform/methanol mixture and evaporating off the solvent. The viscous oil analysed by microanalysis and nuclear magnetic resonance spectroscopy to the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04375472 |
| Source dataset | uspto-grants-1983_03 |
| ORD ID | ord-7a170a13c2544bd194e9399aa7524e56 |
| Source note | uspto-grants-1983_03 |