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

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.

1. temperatureWhen cooled
2. extractionthe aqueous layer was extracted with EtOAc (2×15 mL)
3. washThe combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL)
4. dry with materialdried with NaSO4
5. filtrationfiltered
6. customAfter evaporation of the solvent
7. customlight brown solids were obtained (0.15 g, 62%)
8. customThe compound was used in the next synthetic step without further purification

ORDレコード

ord-4325811208714cde96d7855dd97c1686

出典データセット

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07728016B2