反应详情

温度

120 °C

To a solution of 4,4,5,5-tetramethyl-2-[4-[(1-methylethyl)oxy]-3-(trifluoromethyl)phenyl]-1,3,2-dioxaborolane (D42) (160 mg), 2-bromo-1,3-thiazole (119 mg) and cesium carbonate (237 mg) in acetonitrile (15 mL) and water (3.75 mL) stirred under nitrogen at room temperature was added PdCl2(dppf)-CH2Cl2 adduct (39.6 mg) in one charge. The reaction vessel was sealed and heated under microwave at 120° C. for 1 h. After cooling the reaction, the reaction mixture was filtered and the filtrate was partitioned between ethyl acetate (150 mL) and saturated brine (50 mL). The organic phase was dried over sodium sulphate and evaporated in vacuo. The crude product was purified by column chromatography to give 2-[4-[(1-methylethyl)oxy]-3-(trifluoromethyl)phenyl]-1,3-thiazole (D66) (73 mg). MS (ES): C13H12F3NOS requires 287. found 288.1 (M+H+).

1. additioncharge
2. customThe reaction vessel was sealed
3. temperatureAfter cooling
4. customthe reaction
5. filtrationthe reaction mixture was filtered
6. customthe filtrate was partitioned between ethyl acetate (150 mL) and saturated brine (50 mL)
7. dry with materialThe organic phase was dried over sodium sulphate
8. customevaporated in vacuo
9. customThe crude product was purified by column chromatography