反应 #9993

反应方程式

2-chloro-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine

ethylenediamine

→

2-(2-Amino-ethylamino)-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine

溶剂

ethyl acetate

反应条件

后处理

1. 1
   温度the mixture is heated
2. 2
   温度After cooling to room temperature
3. 3
   萃取extracted with 150 ml of water
4. 4
   萃取The aqueous phase is extracted twice with ethyl acetate
5. 5
   洗涤the combined organic extracts are washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution
6. 6
   干燥dried over magnesium sulfate
7. 7
   过滤After filtration
8. 8
   浓缩the filtrate is concentrated under reduced pressure at 35° C.
9. 9
   其他dried under an HV

实验过程

200 mg (0.58 mmol) of 2-chloro-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine are dissolved in 6 ml (90 mmol) of ethylenediamine and the mixture is heated under reflux for 3 hours (oil bath temperature of 150° C.). After cooling to room temperature, the reaction mixture is taken up in 250 ml of ethyl acetate and extracted with 150 ml of water. The aqueous phase is extracted twice with ethyl acetate and the combined organic extracts are washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution and dried over magnesium sulfate. After filtration, the filtrate is concentrated under reduced pressure at 35° C. and dried under an HV. 2-(2-Amino-ethylamino)-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine is obtained; Rf=0.27 (methylene chloride:methanol:concentrated ammonium hydroxide solution=900:100:1); EI-MS: (M+H)+=346; m.p. 55–56° C.

来源