反应详情

To sodium hydride (220 mg, 55-65% in mineral oil) was added THF (35 ml) followed by addition of 2-phenyl-ethenesulfonic acid [6-(2-hydroxy-ethoxy)-5-p-tolyl-pyrimidin-4-yl]-amide (250 mg). The mixture was stirred for 1 h at rt. Then 5-bromo-2-chloro-pyrimidine (188 mg) was added and stirring continued for 21 h at 80° C. The solvent was evaporated and diethylether (20 ml) was added to the residue. The precipitate was filtered off and washed with diethylether, dissolved in water and acidified by citric acid. The precipitate was filtered off and the crude material was purified by chromatography over silicagel with hexane/EtOAc=1/1 to give 2-phenyl-ethenesulfonic acid {6-[2-(5-bromo-pyrimidin-2-yloxy)-ethoxy]-5-p-tolyl-pyrimidin-4-yl}-amide (91 mg); tR=5.39 (LC); [M+H]+=570.34 (ES+); [M−H]−=568.45 (ES−).

1. stirringstirring
2. waitcontinued for 21 h at 80° C
3. customThe solvent was evaporated
4. additiondiethylether (20 ml) was added to the residue
5. filtrationThe precipitate was filtered off
6. washwashed with diethylether
7. dissolutiondissolved in water
8. filtrationThe precipitate was filtered off
9. customthe crude material was purified by chromatography over silicagel with hexane/EtOAc=1/1