反应详情

温度

100 °C

To a solution of 1-(7-bromo-5-pyridin-3-yl-benzothiazol-2-yl)-3-ethyl-urea (0.125 g, 0.33 mmol) in DMF (5 mL) was added dimethyl-(6-tributylstannanyl-pyridin-2-yl)-amine (0.14 g, 0.33 mmol) under nitrogen atmosphere at room temperature. The reaction mixture was then degassed for half an hour followed by the addition of bis(triphenylphosphine)palladium(II) dichloride (0.023 g, 0.033 mmol). The reaction mixture was then again degassed for half an hour and heated at 100° C. for 15 h under nitrogen atmosphere. After the completion of the reaction (TLC monitoring), DMF was distilled off; water was added to the reaction mixture and extracted with ethyl acetate. The combined organic layers were dried over anhydrous Na2SO4, and evaporated to dryness under reduced pressure. The crude residue was purified by prep HPLC to get the title compound (0.006 g, 5.0%) as off-white solid.

1. customThe reaction mixture was then degassed for half an hour
2. customThe reaction mixture was then again degassed for half an hour
3. customAfter the completion of the reaction (TLC monitoring), DMF
4. distillationwas distilled off
5. additionwater was added to the reaction mixture
6. extractionextracted with ethyl acetate
7. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
8. customevaporated to dryness under reduced pressure
9. customThe crude residue was purified by prep HPLC