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 (xxx) (2 gm, 2.79 mmol) in DMA (5 ml) was added 2,6-lutidine (0.597 g, 5.57 mmol) and 3-(3-aminophenyl)propanamide (intermediate xxvi) (0.915 gm, 5.57 mmole). The reaction mixture was heated at 130° C. for 16 h. The reaction mixture was cooled to room temperature and added water until a solid precipitate was obtained. The solid was filtered, washed with water and small amount of MeOH. The solid was purified by silica gel column chromatography, eluting with DCM:Methanol (9:1), to yield the titled compound (1b) (1.7 g) [m/z=710.20 (M+1)].

1. temperatureThe reaction mixture was cooled to room temperature
2. customwas obtained
3. filtrationThe solid was filtered
4. washwashed with water and small amount of MeOH
5. customThe solid was purified by silica gel column chromatography
6. washeluting with DCM:Methanol (9:1)