反应详情

温度

100 °C

Combine 1-(2-{5-fluoro-4-[7-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzo[b]thiophen-2-yl]-pyrimidin-2-ylamino}-ethyl)-imidazolidin-2-one (120 mg, 0.25 mmol), (6-fluoro-4-iodo-pyridin-3-yl)-methanol (100 mg; 0.32 mmol), (1,1′-bis(di-phenylphosphino)ferrocene)palladium(II) chloride (10.14 mg; 0.01 mmol), 2-(di-tert-butylphosphino)biphenyl (2 mg, 0.01 mmol) and sodium carbonate (2 M, 0.2 mL, 0.4 mmol) in 5 mL of dioxane in a pressure tube. Heat the mixture at 100° C. overnight in oil bath. Cool the mixture down to room temperature, dilute it with chloroform-isopropyl alcohol (3/1). Wash the organic phase with saturated aqueous sodium chloride, dry it over sodium sulfate and concentrate it to an oily residue. Purify the crude by flash column chromatography (10% methanol in dichloromethane) to afford the title compound (25 mg, 21%). MS (ES) m/z 483 [M+1]+.

1. temperatureCool the mixture down to room temperature
2. washWash the organic phase with saturated aqueous sodium chloride
3. dry with materialdry it over sodium sulfate
4. concentrationconcentrate it to an oily residue
5. customPurify the crude by flash column chromatography (10% methanol in dichloromethane)