تفاعل #60071
ord-ccebc15894a44fc982dabfed7783f9fd
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1تركيزThe reaction mixture was concentrated in vacuo
- 2workup.ADDITIONdiluted with water and ethyl acetate
- 3استخلاصThe solution was extracted three times with ethyl acetate
- 4تجفيفdried over sodium sulfate
- 5أخرىpurified by column chromatography
- 6غسيلeluting 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.