Реакция #86410

ord-c197e5073e5441919dd53cab972b80f6

Растворители

Условия реакции

Температура
50°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe reaction mixture was filtered
  2. 2
    Концентрированиеthe filtrate was concentrated in vacuo
  3. 3
    Другоеto give crude product, which
  4. 4
    Другоеwas purified by silica gel column chromatography

Методика

A mixture of 3-(2,6-dichloro-3,5-dimethoxy-phenyl)-1-[6-(2-nitro-phenylamino)-pyrimidin-4-yl]-1-pyridin-3-ylmethyl-urea (85 g, 0.149 mmol) and Fe (84 g, 1.5 mmol) in AcOH (5 mL) was heated at 50° C. for 2 hours. The reaction mixture was filtered and the filtrate was concentrated in vacuo to give crude product, which was purified by silica gel column chromatography to afford the title compound (53 mg, yield: 66%). MS (ESI): 540 [M+H]+.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09434697B2uspto-grants-2016_09