反应 #60071

反应方程式

[5-amino-4-(2,4-dichlorophenyl)pyrimidin-2-yl]{2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}amine

methyliminodiacetic acid

HBTU

N,N-diisopropylethylamine

→

1-[2-({2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}amino)-4-(2,4-dichlorophenyl)pyrimidin-5-yl]-4-methylpiperazine-2,6-dione

反应条件

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 [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.

来源