反应 #60223

ord-bd8920c1d299408e830cf009e8d85e20

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩The reaction mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONdiluted with water and ethyl acetate
  3. 3
    萃取The solution was extracted three times with ethyl acetate
  4. 4
    干燥dried over sodium sulfate
  5. 5
    其他purified by column chromatography
  6. 6
    洗涤eluting with 5-10% methanol/methylene chloride

实验过程

1 mmol of N-[2-({2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}amino)-4-(2,4-dichlorophenyl)pyrimidin-5-yl]acetamide and 2 mmol of Lawesson's reagent were stirred in 2 ml of DME at 80° C. The reaction mixture was concentrated in vacuo and diluted with water and ethyl acetate. The solution was extracted three times with ethyl acetate, dried over sodium sulfate, and purified by column chromatography eluting with 5-10% methanol/methylene chloride.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07425557B2uspto-grants-2008_09