반응 #86410

ord-c197e5073e5441919dd53cab972b80f6

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The reaction mixture was filtered
  2. 2
    농축the filtrate was concentrated in vacuo
  3. 3
    기타to give crude product, which
  4. 4
    기타was purified by silica gel column chromatography

실험 절차

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]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09434697B2uspto-grants-2016_09