反应详情

温度

50 °C

n-Propanesulfonic acid [6-(2-hydroxy-ethoxy)-5-p-tolyl-pyrimidin-4-yl]-amide (115 mg) was dissolved in THF (15 ml). Sodium hydride (60 mg) was added followed by stirring for 15 min at 50° C. Then 2-chloro-5-bromo-pyrimidine (135 mg) was added and stirring was continued for 8 h at 75° C. The reaction mixture was poured onto ice water, acidified with solid citric acid and extracted with ethyl acetate. The combined organic extracts were dried over magnesium sulfate, filtered and the solvent was evaporated. The crude material was purified by plate chromatography with diethyl ether to give n-propanesulfonic acid {6-[2-(5-bromo-pyrimidin-2-yloxy)-ethoxy]-5-p-tolyl-pyrimidin-4-yl}-amide (65 mg) as a white powder. LC-MS: tR: 4.91, [M+H]+: 510.13.

1. stirringstirring
2. waitwas continued for 8 h at 75° C
3. additionThe reaction mixture was poured onto ice water
4. extractionextracted with ethyl acetate
5. dry with materialThe combined organic extracts were dried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent was evaporated
8. customThe crude material was purified by plate chromatography with diethyl ether