Реакция #9993

Уравнение реакции

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

Растворители

ethyl acetate

Условия реакции

Обработка

1. 1
   Температураthe mixture is heated
2. 2
   ТемператураAfter cooling to room temperature
3. 3
   Экстракцияextracted with 150 ml of water
4. 4
   ЭкстракцияThe aqueous phase is extracted twice with ethyl acetate
5. 5
   Промывкаthe combined organic extracts are washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution
6. 6
   Сушкаdried over magnesium sulfate
7. 7
   ФильтрацияAfter filtration
8. 8
   Концентрированиеthe filtrate is concentrated under reduced pressure at 35° C.
9. 9
   Другоеdried under an HV

Методика

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.

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