反应详情

温度

130 °C

To a stirred solution of 1-(2-fluoro-4-iodophenyl)-3-(4-methoxybenzyl)-6,8-dimethyl-2,4,7-trioxo-1,2,3,4,7,8-hexahydropyrido[2,3-d]pyrimidin-5-yl 4-methylbenzene sulfonate (3a) (8.70 gm, 12.13 mmol) in DMA (10 ml) was added 2,6-lutidine (3.5 ml, 30.3 mmol) and methyl 3-aminobenzoate (5.5 g, 36.4 mmol). The reaction mixture was heated at 130° C. for 16 h. The reaction mixture was cooled to room temperature and water was added followed by extraction with Ethyl acetate. The organic phase was dried over sodium sulphate. The solvent was evaporated in vacuo and the residual solid was purified by silica gel column chromatography, eluting with Hexane:Ethyl acetate, to yield the titled compound (3b) (4.2 g)

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionfollowed by extraction with Ethyl acetate
3. dry with materialThe organic phase was dried over sodium sulphate
4. customThe solvent was evaporated in vacuo
5. customthe residual solid was purified by silica gel column chromatography
6. washeluting with Hexane