Reaktion #1943376

Reaktionsgleichung

1-methyl-5-nitroimidazole-2carboxaldehyde

5-ethyl-2-methyl-1,3,4-thiadiazole

→

abovementioned reaction product

2-ethyl-5-[2-(1-methyl-5-nitroimidazol-2-yl)-vinyl]-1,3,4-thiadiazole

Lösungsmittel

acetic acid

acetic anhydride

acetic anhydride

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux temperature for a further 20 hours
2. 2
   Sonstigethe solvent is then evaporated
3. 3
   WaschenThe residue is washed with acetone
4. 4
   WaschenMerck) and eluted with CHCl3 /CH3OH=98 : 2

Vorschrift

A solution of 15.5 g of 1-methyl-5-nitroimidazole-2carboxaldehyde in 50 ml of acetic acid and 25 ml of acetic anhydride is added at reflux temperature over a period of 10 hours to 12.8 g of 5-ethyl-2-methyl-1,3,4-thiadiazole and 0.5 g of ZnCl2 which have been dissolved in 100 ml of acetic acid and 50 ml of acetic anhydride. The mixture is kept at reflux temperature for a further 20 hours and the solvent is then evaporated. The residue is washed with acetone and passed through a ready-to-use silica gel column (Type A of Messrs. Merck) and eluted with CHCl3 /CH3OH=98 : 2. 5.6 g of the abovementioned reaction product with a melting point of 165° C. is obtained; this corresponds to 21% of the theory.

Quelle