反应详情

A stirred solution of 2.1 g of 6-methoxy-2-methyl-4-pyrimidinamine in dry tetrahydrofuran was treated with a solution of 5.4 g of 3-bromo-1-phenyl-1,2-propanedione in 5 ml of dry ether. After stirring overnight, the mixture was chilled and the precipitated salt filtered off. A suspension of the salt in dry ethanol was refluxed for 1.5 hours, chilled, and filtered. The solid was shaken with a mixture of chloroform and aqueous sodium bicarbonate and the organic layer was evaporated to dryness under reduced pressure. The residue was chromatographed in ethyl acetate on silica to obtain 2.7 g of (7-methoxy-5-methyl-imidazo[1,2-c]pyrimidin-2-yl)-phenylmethanone as a yellow crystalline solid melting at 165°-7° C.

1. temperaturethe mixture was chilled
2. filtrationthe precipitated salt filtered off
3. additionA suspension of the salt in dry ethanol
4. temperaturewas refluxed for 1.5 hours
5. temperaturechilled
6. filtrationfiltered
7. stirringThe solid was shaken with a mixture of chloroform and aqueous sodium bicarbonate
8. customthe organic layer was evaporated to dryness under reduced pressure
9. customThe residue was chromatographed in ethyl acetate on silica