反応 #40718

反応方程式

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

溶媒

hydroiodic acid

反応条件

後処理

1. 1
   温度When cooled
2. 2
   抽出the aqueous layer was extracted with EtOAc (2×15 mL)
3. 3
   洗浄The combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL)
4. 4
   乾燥dried with NaSO4
5. 5
   ろ過filtered
6. 6
   その他After evaporation of the solvent
7. 7
   その他light brown solids were obtained (0.15 g, 62%)
8. 8
   その他The compound was used in the next synthetic step without further purification

実験手順

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.

出典