反应 #86410

ord-c197e5073e5441919dd53cab972b80f6

溶剂

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The reaction mixture was filtered
  2. 2
    浓缩the filtrate was concentrated in vacuo
  3. 3
    其他to give crude product, which
  4. 4
    其他was purified by silica gel column chromatography

实验过程

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]+.

来源

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