Réaction #86410

ord-c197e5073e5441919dd53cab972b80f6

Solvants

Conditions de réaction

Température
50°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    FiltrationThe reaction mixture was filtered
  2. 2
    Concentrationthe filtrate was concentrated in vacuo
  3. 3
    Autreto give crude product, which
  4. 4
    Autrewas purified by silica gel column chromatography

Mode opératoire

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]+.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09434697B2uspto-grants-2016_09