反应详情

温度

110 °C

A mixture of ethyl 4-(2-bromo-4-fluorophenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate (3.56 g, 10 mmol) and POCl3 (15 mL) was stirred at 110° C. for 4 hours under N2, then cooled to 25° C. POCl3 was removed in vacuo and the residue was dissolved in chloroform (100 mL). Then the mixture was adjusted to pH 6-8 with strong ammonia. The organic phase was washed with brine (80 mL×3), dried over Na2SO4 and filtered. The filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (PETROLEUM ETHER/EtOAc (V/V)=5/1) to give the title compound as a white solid (1.73 g, 46%). The compound was characterized by the following spectroscopic data:

1. temperaturecooled to 25° C
2. customPOCl3 was removed in vacuo
3. dissolutionthe residue was dissolved in chloroform (100 mL)
4. washThe organic phase was washed with brine (80 mL×3)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationThe filtrate was concentrated in vacuo
8. customThe residue was purified by a silica gel column chromatography (PETROLEUM ETHER/EtOAc (V/V)=5/1)