تفاعل #40718

ord-4325811208714cde96d7855dd97c1686

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةWhen cooled
  2. 2
    استخلاصthe aqueous layer was extracted with EtOAc (2×15 mL)
  3. 3
    غسيلThe combined organic layers were washed with saturated sodium thiosulphate solution (2×15 mL) and brine (20 mL)
  4. 4
    تجفيفdried with NaSO4
  5. 5
    ترشيحfiltered
  6. 6
    أخرىAfter evaporation of the solvent
  7. 7
    أخرىlight brown solids were obtained (0.15 g, 62%)
  8. 8
    أخرىThe compound was used in the next synthetic step without further purification

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728016B2uspto-grants-2010_06