Reaktion #570427

Reaktionsgleichung

3-amino-4-{2-[(5-dimethylaminomethyl-2-furyl)methylthio]ethylamino}-1,2,5-thiadiazole 1-oxide

HCl

→

title compound

Ausbeute 52.0%

N-{2-[(5-Dimethylaminomethyl-2-furyl)methylthio]ethyl}-ethanediimidamide trihydrochloride hydrate

Ausbeute 52.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas warmed slightly
2. 2
   Einengenthe solution was concentrated
3. 3
   Sonstigethe residue was triturated with 70 mL of absolute ethanol
4. 4
   FiltrationThe crystals were collected by filtration
5. 5
   Sonstigedried under vacuum

Vorschrift

A suspension of 3-amino-4-{2-[(5-dimethylaminomethyl-2-furyl)methylthio]ethylamino}-1,2,5-thiadiazole 1-oxide (6.59 g; 20.0 mmoles) [prepared according to published United Kingdom Patent Application No. 2,067,987] in 200 mL of methanol was warmed slightly to achieve complete solution, then treated with 13.3 mL of concentrated HCl. After stirring at ambient temperature for 2.5 hours, the solution was concentrated and the residue was triturated with 70 mL of absolute ethanol. The crystals were collected by filtration and dried under vacuum to give 4.3 g (52%) of the title compound, m.p. 166°-169° C. (dec.).

Quelle