Reacción #86410

ord-c197e5073e5441919dd53cab972b80f6

Disolventes

Condiciones de reacción

Temperatura
50°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónThe reaction mixture was filtered
  2. 2
    Concentraciónthe filtrate was concentrated in vacuo
  3. 3
    Otroto give crude product, which
  4. 4
    Otrowas purified by silica gel column chromatography

Procedimiento

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]+.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09434697B2uspto-grants-2016_09