反应详情

To a suspension of 6-(3-methyl-4-methoxyphenyl)-pyrido[3,2-d]pyrimidin-4(3H)one (1.41 mmole) in toluene (80 ml) was added phosphorus oxychloride (4.23 mmole) and 2,6-lutidine (4.23 mmole). The reaction mixture was refluxed for 16 hours until a black solution was obtained. After evaporation to dryness, the residue was redissolved in ethyl acetate and extracted with a saturated sodium bicarbonate solution. The combined organic layers were evaporated in vacuo. The residue was purified by silica gel column chromatography (the mobile phase being a ethylacetate/hexane mixture in a ratio gradually ranging from 2:8 to 3:7), resulting in the pure title compound (300 mg, yield 74%) which was characterized by its mass spectrum as follows: MS (m/z): 287 ([M+H]+, 100).

1. temperatureThe reaction mixture was refluxed for 16 hours until a black solution
2. customwas obtained
3. customAfter evaporation to dryness
4. dissolutionthe residue was redissolved in ethyl acetate
5. extractionextracted with a saturated sodium bicarbonate solution
6. customThe combined organic layers were evaporated in vacuo
7. customThe residue was purified by silica gel column chromatography (the mobile phase