反应详情

温度

80 °C

A mixture of 4-trifluoromethanesulfonyloxy-5,6-dihydro-2H-pyridine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester (WO 2004/002957; 6.04 g, 15.5 mmol), 2-[3-(2-chloro-3,6-difluoro-phenyl)-isoxazol-5-ylmethoxy]-5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyridine (9.28 g, 20.7 mmol) and aq. 2M Na2CO3 (93.1 mL, 186 mmol) in DME (150 mL) was prepared, and Pd(PPh3)4 (1.00 g, 0.866 mmol) was added in portions. The mixture was heated to 80° C., and stirred at this temperature for 1 h. The mixture was allowed to cool to rt, and was diluted with EtOAc. The resulting mixture was washed with water and brine. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (EtOAc/heptane 1:2→2:1) yielded the title compound (4.64 g, 40%). LC-MS: tR=1.34 min; ES+: 562.34.

1. customwas prepared
2. temperatureto cool to rt
3. washThe resulting mixture was washed with water and brine
4. dry with materiallayer was dried over MgSO4
5. filtrationfiltered
6. customthe solvents were removed under reduced pressure
7. customPurification of the residue by FC (EtOAc/heptane 1:2→2:1)