反应详情

A mixture of 4,5-Bis(diphenylphos-phino)-9,9-dimethylxanthene (xanthopos) (8.6 mg, 0.0148 mmol) and Tris(dibenzylideneacetone)dipalladium(0)[Pd2(dba)3] (6.81 mg, 0.0074 mmol) in dry 1,4-dioxane (5 ml) was stirred vigorously and nitrogen was bubbled through the suspension for 30 minutes. (4-Iodo-phenyl)-(4-methyl-piperazin-1-yl)-methanone (41.1 mg, 0.1247 mmol), 2-Amino-6-(2-methyl-5-nitro-phenyl)-7,8-dihydro-6H-pyrido[4,3-d]pyrimidin-5-one (37.3 mg, 0.1247 mmol) and dry cesium carbonate (100 mg, 0.31 mmol) was added. Nitrogen was bubbled through for another 30 minutes; the mixture was allowed to reflux overnight. The mixture was cooled, diluted with ethylacetate, water was added and the layers were separated. The aqueous layer was extracted with ethyl acetate and the two organic extracts were combined. The organics were washed with brine, then dried (sodium sulfate), filtered and concentrated. Silica gel chromatography using 5-10% ethyl acetate/hexane as eluent provided 6-(2-Methyl-5-nitro-phenyl)-2-[4-(4-methyl-piperazine-1-carbonyl)phenylamino]-7,8-dihydro-6H-pyrido[4,3-d]pyrimidin-5-one [22] as a yellow solid [Yield: 12.3 mg, 19.7%]

1. customnitrogen was bubbled through the suspension for 30 minutes
2. customNitrogen was bubbled through for another 30 minutes
3. temperatureto reflux overnight
4. temperatureThe mixture was cooled
5. additiondiluted with ethylacetate, water
6. additionwas added
7. customthe layers were separated
8. extractionThe aqueous layer was extracted with ethyl acetate
9. washThe organics were washed with brine
10. dry with materialdried (sodium sulfate)
11. filtrationfiltered
12. concentrationconcentrated