تفاعل #60095

ord-00194101e6bb4772933de5df17d9fb70

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 [5-amino-4-(2,4-dichlorophenyl)pyrimidin-2-yl]{2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}amine and 1 mmol of acetic anhydride were stirred at room temperature for four hours in THF. 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 N-[2-({2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}amino)-4-(2,4-dichlorophenyl)pyrimidin-5-yl]acetamide.

المصدر

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