反应详情

温度

85 °C

A mixture of (4-{[4-difluoromethoxy-2-ethyl-8-fluoro-5-(2-methoxy-2-oxoethoxy)quinolin-3-yl]methyl}phenyl)boronic acid (0.15 g), 4-bromo-5-cyclopropylisoxazole (0.24 g), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium (0.027 g), sodium hydrogen carbonate (0.082 g), 1,2-dimethoxyethane (1.0 mL) and water (0.4 mL) was heated at 85° C. for 2 hours. The mixture was cooled to room temperature, diluted with water (5 mL), neutralised by the addition of 1.0 M aqueous hydrochloric acid solution (1.0 mL) and extracted with ethyl acetate. The combined extracts were washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and then concentrated under reduced pressure. Purification of the residue by column chromatography on silica gel, eluting with a mixture of cyclohexane and ethyl acetate (1:0 to 7:3 by volume) gave title compound as a colourless oil (0.03 g).

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. washThe combined extracts were washed with saturated aqueous sodium chloride solution
4. dry with materialdried over magnesium sulphate
5. concentrationconcentrated under reduced pressure
6. customPurification of the residue by column chromatography on silica gel
7. washeluting with a mixture of cyclohexane and ethyl acetate (1:0 to 7:3 by volume)