反応 #9993

反応方程式

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

溶媒

ethyl acetate

反応条件

後処理

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

実験手順

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.

出典