反应详情

5-bromo-2-iodopyrimidine (0.320 g), 4-(trifluoromethyloxy)phenylboronic acid (FRONTIER SCIEN., 0.231 g), tetrakis(triphenylphosphine)palladium(0) (ALDRICH, 0.026 g) and sodium carbonate (1.6 ml, 2M in H2O) in dry toluene (2.8 ml) was refluxed for 24 hours under argon atmosphere. After cooling to room temperature, H2O (5 ml) was added to the reaction mixture. The layers were separated and the aqueous layer was extracted with CH2Cl2 (3×15 ml). The combined organic layers were washed with brine, dried over MgSO4, concentrated under vacuum and purified by column chromatography on silica gel, eluting with EtOAc-hexane 1:20 to give 0.248 g of the desired product as a white solid.

1. customThe layers were separated
2. extractionthe aqueous layer was extracted with CH2Cl2 (3×15 ml)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated under vacuum
6. custompurified by column chromatography on silica gel
7. washeluting with EtOAc-hexane 1:20