反应详情

温度

100 °C

To a solution of 5-bromo-6-(2, 2, 2-trifluoro-ethoxy)-pyridin-3-ylamine (2.1 g, 7.74 mmol) in DME, ethanol, water (3:1:1) (50 ml) in a sealed tube were added 4-chlorophenylboronic acid (CAS Registry No. 1679-18-1) (1.8 g, 11.62 mmol) and potassium phosphate (4.9 g, 23.22 mmol), and then the reaction mixture was purged with nitrogen for 15 min. Then Pd(dppf)2Cl2 (651 mg, 0.93 mmol) was added to the reaction mixture and heated at 100° C. for 4 h. The reaction mixture was filtered off and the filter cake was washed with ethyl acetate (3×20 ml). The organic layer was washed with water, brine, dried over Na2SO4 and evaporated in vacuo to get the crude (1.9 g). The crude was purified by column chromatography (20-25% ethyl acetate/hexane) to get the desired product (1.3 g, 56%) as brown liquid. MS (LC/MS): 303.0 (M+H).

1. filtrationThe reaction mixture was filtered off
2. washthe filter cake was washed with ethyl acetate (3×20 ml)
3. washThe organic layer was washed with water, brine
4. dry with materialdried over Na2SO4
5. customevaporated in vacuo
6. customto get the crude (1.9 g)
7. customThe crude was purified by column chromatography (20-25% ethyl acetate/hexane)