تفاعل #60071

ord-ccebc15894a44fc982dabfed7783f9fd

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 [5-amino-4-(2,4-dichlorophenyl)pyrimidin-2-yl]{2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}amine, and 2 mmol of methyliminodiacetic acid, 4 mmol of HBTU, and 5 mmol of N,N-diisopropylethylamine were added to solution and stirred for six hours at room temperature. 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 1-[2-({2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}amino)-4-(2,4-dichlorophenyl)pyrimidin-5-yl]-4-methylpiperazine-2,6-dione.

المصدر

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