HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Chloride → N-Methoxy-N'-methyl-N"-[2-((4-methyl-5-imidazolyl)methylthio)ethyl]guanidine dihydrochloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Chloride | HCID 5234 | — |
| Edukt | Potassium Bicarbonate | HCID 516893 | — |
| Edukt | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Edukt | HCID 178485010 | HCID 178485010 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | N-Methoxy-N'-methyl-N"-[2-((4-methyl-5-imidazolyl)methylthio)ethyl]guanidine dihydrochloride | HCID 178485009 | 72,5% |
Reaktionsschritte
A mixture of the isothiourea dihydrochloride from Example I (i) (6.6 g), methoxyamine hydrochloride (5.0 g), potassium hydrogen carbonate (8.0 g) and water (60 ml) was refluxed for 24 hours. Following cooling, an excess of sodium chloride was added and the solution extracted with chloroform (5×100 ml). The chloroform extracts were concentrated to give the free base which was purified on a column of silica gel by elution with chloroform-methanolic ammonia. After treatment with an excess of ethanolic hydrogen chloride, the residue was triturated with acetonitrile to give the title compound (2.5 g), m.p. 182°-185°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04034101 |
| Quelldatensatz | uspto-grants-1977_07 |
| ORD ID | ord-86b0d2634dc841e2af52fb5200316428 |
| Quellennotiz | uspto-grants-1977_07 |