Реакция #9990

Уравнение реакции

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

ethylenediamine

→

2-(2-Amino-ethyl-amino)-6-(3-chloro-phenylamino)-9-ethyl-9H-purine

Растворители

ethyl acetate

Условия реакции

Обработка

1. 1
   Температураthe solution is heated
2. 2
   ТемператураAfter cooling to room temperature
3. 3
   Экстракцияextracted with water (150 ml)
4. 4
   ЭкстракцияThe aqueous phase is extracted twice with ethyl acetate
5. 5
   Промывкаthe combined organic extracts are washed successively 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
   Другоеthe residue is dried under an HV
10. 10
    ДругоеThe crude product is recrystallized from diethyl ether

Методика

250 mg (0.81 mmol) of 2-chloro-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine are dissolved in 5.8 ml (97 mmol) of ethylenediamine and the solution 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 ethyl acetate (250 ml) and extracted with water (150 ml). The aqueous phase is extracted twice with ethyl acetate and the combined organic extracts are washed successively 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 the residue is dried under an HV. The crude product is recrystallized from diethyl ether. 2-(2-Amino-ethyl-amino)-6-(3-chloro-phenylamino)-9-ethyl-9H-purine is obtained; Rf=0.22 (methylene chloride:methanol:concentrated aqueous ammonium hydroxide solution=900:100:1); FAB-MS: (M+H)+=322; m.p. 79–80° C.

Источник