反应详情

To a solution of 2-(6-amino-5-bromopyrimidin-4-yloxy)ethanol (611 mg) in dimethylformamide (20 ml) is added sodium hydride (60% dispersion-type, 125 mg), and the mixture is stirred for 20 minutes. To the mixture is added 2-chloro-5-methylthiopyrimidine (461 mg), and the mixture is stirred at room temperature for three hours. To the mixture is added ice-water, and the mixture is extracted with ethyl acetate. The ethyl acetate layer is washed, dried, and evaporated to remove the solvent. The residue is purified by silica get column chromatography (solvent; chloroform/methanol=20:1), and crystallized from ethyl acetate/diisopropyl ether to give 5-bromo-6-[2-(5-methythiopyrimidin-2-yloxy)ethoxy]pyrimidine-4-amine (501 mg).

1. stirringthe mixture is stirred at room temperature for three hours
2. extractionthe mixture is extracted with ethyl acetate
3. washThe ethyl acetate layer is washed
4. customdried
5. customevaporated
6. customto remove the solvent
7. customThe residue is purified by silica
8. customget column chromatography (solvent; chloroform/methanol=20:1)
9. customcrystallized from ethyl acetate/diisopropyl ether