Reaktion #86410

ord-c197e5073e5441919dd53cab972b80f6

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

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]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434697B2uspto-grants-2016_09