Reaktion #573192

Reaktionsgleichung

7-amino-2-(2-furyl)-5-[4-methoxyphenyl][1,2,4]triazolo[1,5-a][1,3,5]triazine

acetic anhydride

→

7-acetylamino-2-(2-furyl)-5-[4-methoxyphenyl][1,2,4]triazolo[1,5-a][1,3,5]triazine

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was then evaporated in vacuo
2. 2
   Sonstigethe residue was purified by chromatography on silica-gel
3. 3
   Wascheneluting with dichloromethane
4. 4
   workup.ADDITIONcontaining ethyl acetate (5% v/v)
5. 5
   SonstigeThe solid obtained from the chromatography
6. 6
   Sonstigewas crystallised from ethanol

Vorschrift

A solution of 7-amino-2-(2-furyl)-5-[4-methoxyphenyl][1,2,4]triazolo[1,5-a][1,3,5]triazine (0.23 g) in acetic anhydride (10 ml) was heated on the steam-bath for 18 hours. The solvent was then evaporated in vacuo and the residue was purified by chromatography on silica-gel eluting with dichloromethane containing ethyl acetate (5% v/v). The solid obtained from the chromatography was crystallised from ethanol and gave 7-acetylamino-2-(2-furyl)-5-[4-methoxyphenyl][1,2,4]triazolo[1,5-a][1,3,5]triazine m.p. 243°-6° C.; microanalysis, found: C, 58.0; H, 4.0; N, 23.9% C17H14N6O3 requires C, 58.3; H, 4.0; N, 24.0%; NMR 2.50 (s, NHCOCH3), 3.87 (s, 3H, CH3O), 6.75 (d of d, 1H, furyl-4H), 7.12 and 8.42 (A2B2 pattern, 4H, phenyl-H), 7.32 (d, 1H, furyl-3H), 7.98 (d, 1H, furyl-5H) and 11.42 (s, H, NHCOCH); m/e 351 (M+H)+.

Quelle