反应详情

温度

0 °C

2-(2-Chloro-4-nitrophenyl)-N-methoxyacetamide (49.3 mmol) and 4-chloro-2-(methylthio)pyrimidine-5-carbaldehyde (41.2 mmol) were dissolved in DMF (600 mL). The solution was cooled to 0° C., and K2CO3 (91 mmol) was added in one poroom temperatureion. The mixture was stirred at 0° C. for 2 h and then at room temperature for 48 h. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure to 60 mL. Water (600 mL) was added. The precipitate was filtered, washed twice with EtOH and dried. The by-product (Z) -6-(2-chloro-4-nitrophenyl)-2-(methylthio)-7H-pyrano[2,3-d]pyrimidin-7-one O-methyl oxime was separated by reflux of the mixture for 4 h in EtOH and hot filtration of the suspension through a sintered glass funnel. Evaporation of the filtrate and drying gave 6-(2-chloro-4-nitrophenyl)-8-methoxy-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one as a solid (63%).

1. waitat room temperature for 48 h
2. filtrationThe reaction mixture was filtered
3. concentrationthe filtrate was concentrated under reduced pressure to 60 mL
4. additionWater (600 mL) was added
5. filtrationThe precipitate was filtered
6. washwashed twice with EtOH
7. customdried
8. customThe by-product (Z) -6-(2-chloro-4-nitrophenyl)-2-(methylthio)-7H-pyrano[2,3-d]pyrimidin-7-one O-methyl oxime was separated
9. temperatureby reflux of the mixture for 4 h in EtOH
10. filtrationhot filtration of the suspension through a sintered glass funnel
11. customEvaporation of the filtrate
12. customdrying