反应详情

A mixture of 0.60 g (2 mmol) of 5-amino-4-(methylamino)-2-[[4-(morpholin-4-yl)phenyl]amino]pyrimidine, 0.74 g (3 mmol) ethyl 2-(2,6-dichlorophenyl)-2-oxoacetate (T. H. Kress and M. R. Leanna, Synthesis, 1988:803–805), and 0.3 mL HOAc in 25 mL of 2-methoxyethanol is heated under reflux for 16 hours before the solvent is removed under vacuum. The residue is extracted into EtOAc and, after being washed with water, the solution is dried over Na2SO4. Removal of the solvent and chromatography on silica, eluting with hexane/EtOAc 3:2 gives 0.36 g (37%) of the title compound (Compound 2 in Tables 1 and 2): mp (EtOH) 292–293° C.

1. temperatureis heated
2. temperatureunder reflux for 16 hours before the solvent
3. customis removed under vacuum
4. extractionThe residue is extracted into EtOAc
5. washafter being washed with water
6. dry with materialthe solution is dried over Na2SO4
7. customRemoval of the solvent and chromatography on silica
8. washeluting with hexane/EtOAc 3:2