Реакция #9994

Уравнение реакции

2-chloro-6-(3-chloro-phenyl-amino)-purine

caesium carbonate

isopropyl iodide

→

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

Растворители

ethyl acetate

DMF water

dioxane

Условия реакции

Обработка

1. 1
   workup.ADDITIONare added at room temperature
2. 2
   Другоеthe reaction to completion
3. 3
   workup.STIRRINGthe reaction mixture is stirred at 45° C. for a further 24 hours
4. 4
   Промывкаwashed with water (2 times) and saturated sodium chloride solution
5. 5
   Сушкаdried over magnesium sulfate
6. 6
   ФильтрацияAfter filtration
7. 7
   Концентрированиеthe filtrate is concentrated under reduced pressure at 35° C.
8. 8
   Другоеthe residue is dried under an HV
9. 9
   ДругоеThe resulting crude product is purified by crystallization from diethyl ether/hexane

Методика

500 mg (1.78 mmol) of 2-chloro-6-(3-chloro-phenyl-amino)-purine are dissolved in a mixture of 29.5 ml of DMF/water (85/15) and 5 ml of dioxane by means of gentle heating. 870 mg (2.67 mmol) of caesium carbonate, followed by 1.78 ml (17.8 mmol) of isopropyl iodide are added at room temperature. The reaction mixture is stirred at room temperature for 18 hours. To bring the reaction to completion, the reaction mixture is stirred at 45° C. for a further 24 hours. When the reaction has ended, the reaction mixture is diluted with ethyl acetate, washed with water (2 times) 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 resulting crude product is purified by crystallization from diethyl ether/hexane. 2-Chloro-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine is obtained; Rf=0.46 (ethyl acetate); m.p. 128–129° C.

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