反応 #86410

ord-c197e5073e5441919dd53cab972b80f6

溶媒

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The reaction mixture was filtered
  2. 2
    濃縮the filtrate was concentrated in vacuo
  3. 3
    その他to give crude product, which
  4. 4
    その他was purified by silica gel column chromatography

実験手順

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]+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09434697B2uspto-grants-2016_09