تفاعل #60096

معادلة التفاعل

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

Lawesson's reagent

→

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

المذيبات

DME

ظروف التفاعل

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 N-[2-({2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}amino)-4-(2,4-dichlorophenyl)pyrimidin-5-yl]acetamide and 2 mmol of Lawesson's reagent were stirred in 2 ml of DME at 80° C. 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]amino}ethane-1-thione.

المصدر