Reaktion #9993

Reaktionsgleichung

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

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture is heated
2. 2
   TemperaturAfter cooling to room temperature
3. 3
   Extraktionextracted with 150 ml of water
4. 4
   ExtraktionThe aqueous phase is extracted twice with ethyl acetate
5. 5
   Waschenthe combined organic extracts are washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution
6. 6
   Trocknendried over magnesium sulfate
7. 7
   FiltrationAfter filtration
8. 8
   Einengenthe filtrate is concentrated under reduced pressure at 35° C.
9. 9
   Sonstigedried under an HV

Vorschrift

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.

Quelle