反应详情

温度

100 °C

A mixture of [3-(4-bromobenzyl)-4-difluoromethoxy-2-ethyl-8-fluoroquinolin-5-yloxy]acetic acid methyl ester (0.40 g), carbamic acid tert-butyl ester (0.19 g), tris(dibenzylideneacetone)dipalladium(0) (0.073 g), Xantphos (0.014 g), cesium carbonate (0.58 g) and 1,4-dioxane (5.0 mL) was heated at 100° C. for 10 hours. The mixture was cooled to room temperature, acidified by the addition of glacial acetic acid and partitioned between ethyl acetate and water. The organic phase was dried over magnesium sulfate and concentrated under reduced pressure. Purification of the residue by column chromatography on silica gel, eluting with a mixture of dichloromethane and ethyl acetate (1:0 to 10:1 by volume) gave title compound as a yellow gum (0.11 g).

1. temperatureThe mixture was cooled to room temperature
2. custompartitioned between ethyl acetate and water
3. dry with materialThe organic phase was dried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customPurification of the residue by column chromatography on silica gel
6. washeluting with a mixture of dichloromethane and ethyl acetate (1:0 to 10:1 by volume)