Reaktion #40718

Reaktionsgleichung

water

1-(5-Chloro-2,4-dimethoxy-phenyl)-5-(4-fluoro-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid

acetic acid

acetic anhydride

→

1-(2,4-Dihydroxy-phenyl)-5-(4-fluoro-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid

Lösungsmittel

hydroiodic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturWhen cooled
2. 2
   Extraktionthe aqueous layer was extracted with EtOAc (2×15 mL)
3. 3
   WaschenThe combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL)
4. 4
   Trocknendried with NaSO4
5. 5
   Filtrationfiltered
6. 6
   SonstigeAfter evaporation of the solvent
7. 7
   Sonstigelight brown solids were obtained (0.15 g, 62%)
8. 8
   SonstigeThe compound was used in the next synthetic step without further purification

Vorschrift

1-(5-Chloro-2,4-dimethoxy-phenyl)-5-(4-fluoro-phenyl)-1H-[1,2,3]triazole-4-carboxylic acid (0.29 g, 0.77 mmol) was refluxed in a mixture of hydroiodic acid (5 mL), acetic acid (1 mL) and acetic anhydride (0.5 mL) for 16 hours. When cooled, water (20 mL) was added and the aqueous layer was extracted with EtOAc (2×15 mL). The combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL), dried with NaSO4 and filtered. After evaporation of the solvent, light brown solids were obtained (0.15 g, 62%). The compound was used in the next synthetic step without further purification.

Quelle