反应详情

1.0 g (5.29 mmol) of 2,6-dichloro-purine is dissolved in DMF (20 ml) and treated with 152 mg (80%, 5.3 mmol) of sodium hydride and the mixture is stirred at RT for 0.5 hours. After addition of 0.42 ml (5.3 mmol) of ethyl iodide, the mixture is stirred at 70° C. for 3 hours, diluted with ethyl acetate (100 ml) and extracted with concentrated brine. The organic phase is dried (sodium sulfate) and concentrated and the residue is chromatographed (silica gel, methylene chloride:methanol=19:1). An oily mixture comprising 2,6-dichloro-7-ethyl-7H-purine and 2,6-dichloro-9-ethyl-9H-purine is obtained.

1. stirringthe mixture is stirred at 70° C. for 3 hours
2. extractionextracted with concentrated brine
3. dry with materialThe organic phase is dried (sodium sulfate)
4. concentrationconcentrated
5. customthe residue is chromatographed (silica gel, methylene chloride:methanol=19:1)