反应详情

温度

105 °C

A mixture of 4-chloro-5-iodo-7-isopropylpyrrolo[2,3-d]pyrimidine (0.57 g), 4-nitrophenylboronic acid (0.30 g), bis(triphenylphosphine)palladium (II) chloride (0.126 g), toluene (15 ml), ethanol (2 ml), water (4 ml) and sodium bicarbonate (0.45 g) was heated under nitrogen at 105° C. for 8 hours. The mixture was cooled to ambient temperature and then partitioned between brine (50 ml) and ethyl acetate (50 ml). The aqueous layer was further extracted with ethyl acetate and the combined ethyl acetate extracts were washed with water, dried, filtered and evaporated to leave a solid which was purified by flash column chromatography on silica using cyclohexane with increasing amounts of ethyl acetate as the mobile phase to give 4-chloro-7-isopropyl-5-(4-nitrophenyl)pyrrolo[2,3-d]pyrimidine.

1. temperatureThe mixture was cooled to ambient temperature
2. custompartitioned between brine (50 ml) and ethyl acetate (50 ml)
3. extractionThe aqueous layer was further extracted with ethyl acetate
4. washthe combined ethyl acetate extracts were washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customto leave a solid which
9. customwas purified by flash column chromatography on silica