反应详情

温度

140 °C

The mixture of rac-cis-(2-bromo-5-methylphenyl)(3-methyl-2-(((5-(trifluoromethyl)pyridin-2-yl)amino)methyl)piperidin-1-yl)methanone (0.03 g, 0.0638 mmol), 2-(tributylstannyl)pyrimidine (0.028 g, 0.0766 mmol), P(PPh3)4 (0.011 g, 0.01 mmol), Cs2CO3 (0.42 g, 0.13 mmol) and dioxane (1 mL) was degassed for 5 min and heated overnight at 140° C. oil bath. The completion of reaction was monitored by analytical HPLC. The mixture was cooled and extracted with EtOAc. The combine organic layers were washed with saturated NaHCO3 and dried over Na2SO4. The solvent was removed in vacuo to obtain the crude, which was purified by preparative-HPLC to obtain the title compound as TFA salt. ESI-MS (m/z): 470, [M+1]+.

1. customwas degassed for 5 min
2. customThe completion of reaction
3. temperatureThe mixture was cooled
4. extractionextracted with EtOAc
5. washThe combine organic layers were washed with saturated NaHCO3
6. dry with materialdried over Na2SO4
7. customThe solvent was removed in vacuo
8. customto obtain the crude, which
9. customwas purified by preparative-HPLC