Реакция #1350575

ord-d173def10ff74d839ab2941e41693da7

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), 3-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 (12 mg, 26%). Rf 0.41 (ethyl acetate-toluene, 1:1).

Источник

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