Реакция #1350577

ord-aa367d762c4e4395ad45c48edad4149f

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Промывкаthe organic layer washed with further brine
  2. 2
    Сушкаdried over magnesium sulphate
  3. 3
    Концентрированиеconcentrated in vacuo
  4. 4
    ДругоеThe crude product was purified by column chromatography (ethyl acetate-toluene, 1:1)

Методика

A mixture of 3-(3-aminophenyl)-4-bromo-1-methylpyrazole (30 mg, 0.12 mmol), 2-fluorophenylacetic acid (18 mg, 0.12 mmol), 1-hydroxybenzotriazole hydrate (16 mg, 0.12 mmol) and 2-(1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium hexafluoro-phosphate (46 mg, 0.12 mmol) were dissolved in chloroform (1.5 ml). N, N-Diisopropylethylamine (0.02 ml, 0.13 mmol) was added and the mixture stirred at room temperature for 16 h. The reaction mixture was then poured into brine and the organic layer washed with further brine, dried over magnesium sulphate and then concentrated in vacuo. The crude product was purified by column chromatography (ethyl acetate-toluene, 1:1), giving the title compound (15 mg, 32%). Rf 0.52 (ethyl acetate-toluene, 1:1).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06541209B1uspto-grants-2003_04