反应详情

温度

130 °C

To a solution of {1-[2-bromo-4-(pyridine-4-ylcarbamoyl)-phenyl]-ethyl}-carbamic acid tert-butyl ester (2087 μmol) and 3-hydroxyphenylboronic acid (1.55 eq) in a mixture of DME/EtOH: 1/1 (8 ml) were added Na2CO3 (4 eq) and Pd tetrakis (0.05 eq.). The reaction mixture was flushed with Ar and was heated in the microwave at 130° C. for 1.5 hours. The reaction mixture was cooled to RT, diluted with 1N NaHCO3 and extracted with EtOAc. The organic layer was extracted with 1N NaHCO3 and the combined aqueous layers were acidified with citric acid and 1N HCl. The aqueous layer was extracted with EtOAc, the organic layer was dried over MgSO4 and the solvent was removed under reduced pressure. The compound was purified by recrystallization from EtOAc.

1. customThe reaction mixture was flushed with Ar
2. temperatureThe reaction mixture was cooled to RT
3. additiondiluted with 1N NaHCO3
4. extractionextracted with EtOAc
5. extractionThe organic layer was extracted with 1N NaHCO3
6. extractionThe aqueous layer was extracted with EtOAc
7. dry with materialthe organic layer was dried over MgSO4
8. customthe solvent was removed under reduced pressure
9. customThe compound was purified by recrystallization from EtOAc