反应详情

温度

90 °C

To a suspension of 2-{2-[7-chloro-3-(3,5-dimethylphenyl)-6-iodo-2-oxo -1,2-dihydroquinolin-4-yloxy]-ethyl}-piperidine-1-carboxylic acid tert-butyl ester (0.10 g in a mixture of 1 mL N,N-dimethylformamide and 0.04 mL triethylamine) was added 75 mg of 4-aminopyrimidine followed by 0.8 mg dichlorobis(triphenylphosphine)palladium(II) and the flask flushed (5×) with carbon monoxide. The mixture was then heated to 90° C. on an oil bath under a carbon monoxide atmosphere. After 16 hours, the mixture was cooled to room temperature, diluted with ethyl acetate and washed with water and brine. The organic portion was dried over sodium sulfate and concentrated in vacuo. Purification by flash chromatography on silica gel (ethyl acetate:hexane, 35:65; then methylene chloride:methanol, 95:5) gave the title compound (70 mg).

1. customthe flask flushed (5×) with carbon monoxide
2. temperaturethe mixture was cooled to room temperature
3. additiondiluted with ethyl acetate
4. washwashed with water and brine
5. dry with materialThe organic portion was dried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customPurification by flash chromatography on silica gel (ethyl acetate