반응 #40718

반응 방정식

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

용매

hydroiodic acid

반응 조건

후처리

1. 1
   온도When cooled
2. 2
   추출the aqueous layer was extracted with EtOAc (2×15 mL)
3. 3
   세척The combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL)
4. 4
   건조dried with NaSO4
5. 5
   여과filtered
6. 6
   기타After evaporation of the solvent
7. 7
   기타light brown solids were obtained (0.15 g, 62%)
8. 8
   기타The compound was used in the next synthetic step without further purification

실험 절차

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.

출처