反应详情

Under an argon atmosphere, N-(4-iodophenyl)pyrimidin-2-amine (75 mg) was added to a suspension of sodium hydride (16 mg) in anhydrous DMF (3 ml), and the resulting mixture was stirred at room temperature for 30 minutes. The reaction solution was cooled to 0° C. and benzyl bromide (0.039 ml) was added thereto, followed by stirring the resulting mixture at room temperature for 1 hour. Saturated brine was added to the reaction solution and the resulting mixture was extracted 3 times with ethyl acetate. Organic layers were washed 3 times with water and dried over anhydrous sodium sulfate. After removing anhydrous sodium sulfate by filtration, the filtrate was concentrated. The residue was purified by column chromatography (silica gel, eluent:ethyl acetate/hexane=1/15) to obtain N-benzyl-N-(4-iodophenyl)pyrimidin-2-amine (67 mg).

1. temperatureThe reaction solution was cooled to 0° C.
2. stirringby stirring the resulting mixture at room temperature for 1 hour
3. extractionthe resulting mixture was extracted 3 times with ethyl acetate
4. washOrganic layers were washed 3 times with water
5. dry with materialdried over anhydrous sodium sulfate
6. customAfter removing anhydrous sodium sulfate
7. filtrationby filtration
8. concentrationthe filtrate was concentrated
9. customThe residue was purified by column chromatography (silica gel, eluent:ethyl acetate/hexane=1/15)