تفاعل #60126

ord-25669a844f034f04b49514e88526da2a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe reaction mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONdiluted with water and ethyl acetate
  3. 3
    استخلاصThe solution was extracted three times with ethyl acetate
  4. 4
    تجفيفdried over sodium sulfate
  5. 5
    أخرىpurified by column chromatography
  6. 6
    غسيلeluting with 5-10% methanol/methylene chloride

الإجراء التجريبي

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 to obtain {2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}[6-(2,4-dichlorophenyl)-5-nitro(2-pyridyl)]amine.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425557B2uspto-grants-2008_09