Reaktion #1444737

Reaktionsgleichung

2-amino-2-cyanoacetamide

ethyl acetimidate hydrochloride

n-propylamine

→

title compound

Ausbeute 45.2%

5-Amino-2-methyl-1-n-propylimidazole-4-carboxamide

Ausbeute 45.2%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled to 0° C.
2. 2
   workup.STIRRINGstirred for a further hour
3. 3
   FiltrationThe reaction mixture was filtered
4. 4
   workup.STIRRINGThe solution was stirred at room temperature for an hour
5. 5
   workup.WAITleft
6. 6
   FiltrationThe resulting precipitate was filtered
7. 7
   Waschenwashed with acetonitrile
8. 8
   Trocknendichloromethane and dried under vacuum

Vorschrift

A mixture of 2-amino-2-cyanoacetamide (prepared as described in WO 94/00453; 3.6 g, 36.4 mmol) and ethyl acetimidate hydrochloride (4.50 g, 36.4 mmol) in acetonitrile (85 mL) was stirred at 50° C. for an hour, then cooled to 0° C., and stirred for a further hour. The reaction mixture was filtered, and n-propylamine (3.02 mL, 36.4 mmol) added. The solution was stirred at room temperature for an hour, and left to stand for a further 16 hours. The resulting precipitate was filtered, washed with acetonitrile, then dichloromethane and dried under vacuum to afford the title compound as a solid (3.0 g, 45%).

Quelle