反应详情

温度

80 °C

A solution of 0.84 g (1.2 mmol) bis(triphenylphosphine)palladium(II)chloride, 9.58 g (40 mmol) methyl 6-chloro-4-(trifluoromethyl)nicotinate and 10.08 g (52 mmol) of 4-(trifluoromethyl)benzeneboronic acid in 200 ml degassed toluene was treated with 40 ml aqueous 2M K3PO4 and heated at 80° C. for 16 h. The reaction was cooled to RT and extracted with H2O (0° C.)/Et2O (3x). The organic phases were washed with aqueous 10% NaCl, dried (NaSO4) and evaporated. Purification by flash-chromatography on silica gel (dichloromethane/heptane 2:1 to 1:1) gave 9.91 g of the title compound as an off-white powder.

1. temperatureThe reaction was cooled to RT
2. extractionextracted with H2O (0° C.)/Et2O (3x)
3. washThe organic phases were washed with aqueous 10% NaCl
4. dry with materialdried (NaSO4)
5. customevaporated
6. customPurification by flash-chromatography on silica gel (dichloromethane/heptane 2:1 to 1:1)