反应详情

温度

50 °C

Ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-p-tolyl-pyrimidin-4-yl]-amide (135 mg) was dissolved in THF (15 ml) and sodium hydride (80 mg) was added followed by stirring for 15 min at 50° C. Then 2-chloro-5-bromo-pyrimidine (162 mg) was added and stirring was continued for 8 h at 70 C. The reaction mixture was poured onto ice water, acidified with solid citric acid and extracted with ethylacetate. The combined organic extracts were dried over magnesium sulfate and the solvent was evaporated. The crude material was purified by plate chromatography with ethyl acetate/hexane=½ to give ethanesulfonic acid {6-[2-(5-bromo-pyrimidin-2-yloxy)-ethoxy]-5-p-tolyl-pyrimidin-4-yl}-amide (68 mg) as a white powder. LC-MS: tR: 4.64, [M+H]+: 496.19.

1. stirringstirring
2. waitwas continued for 8 h at 70 C
3. additionThe reaction mixture was poured onto ice water
4. extractionextracted with ethylacetate
5. dry with materialThe combined organic extracts were dried over magnesium sulfate
6. customthe solvent was evaporated
7. customThe crude material was purified by plate chromatography with ethyl acetate/hexane=½