反应 #60226

ord-540f91fafa474bc3b55d882a4392de1f

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 2-(2,4-dichlorophenyl)-6-chloro-3-nitropyridine was taken with 2 mmol of (2-aminoethyl)(6-amino-5-nitro(2-pyridyl))amine and 3 mmol of N,N-diisopropylethylamine in 2 ml of DMF at 80° C. for two hours. 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