反应详情

676 mg (2.413 mmol) of 2-chloro-6-(3-chloro-phenyl-amino)-purine are dissolved in 10 ml of abs. DMF by means of gentle heating. 375 mg (2.713 mmol) of potassium carbonate, followed by 0.97 ml (12.01 mmol) of ethyl iodide are added at room temperature. The reaction mixture is stirred at room temperature for 2 hours. When the reaction is complete, the reaction mixture is poured onto ice/water (60 ml) and stirred for 10 minutes. The inhomogeneous mixture is extracted three times with ethyl acetate. The combined organic extracts are washed twice with water and once with 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. The resulting crude product (crystalline oil) is purified by crystallization from diethyl ether/hexane. 2-Chloro-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine is obtained; Rf=0.55 (ethyl acetate:hexane=3:1); APCI-MS: (M+H)+=308; HPLC: tret(grad 20/1)=12.40 minutes; m.p. 127–128° C.

1. additionare added at room temperature
2. additionthe reaction mixture is poured onto ice/water (60 ml)
3. stirringstirred for 10 minutes
4. extractionThe inhomogeneous mixture is extracted three times with ethyl acetate
5. washThe combined organic extracts are washed twice with water and once with saturated sodium chloride solution
6. dry with materialdried over magnesium sulfate
7. filtrationAfter filtration
8. concentrationthe filtrate is concentrated under reduced pressure at 35° C.
9. customdried under an HV
10. customThe resulting crude product (crystalline oil) is purified by crystallization from diethyl ether/hexane