反应详情

温度

200 °C

To a 500 mL 3-neck round bottom flask was added 3-(1-phenyl-1H-imidazol-2-yl)phenol (3.05 g, 12.26 mmol), 2-(3-iodophenyl)-1-phenyl-1H-imidazole (4.67 g, 13.49 mmol), picolinic acid (2.27 g, 18.40 mmol), copper(I) iodide (0.70 g, 3.68 mmol), potassium phosphate tribasic monohydrate (9.88 g, 42.9 mmol), and 200 mL DMSO. Nitrogen was bubbled directly into the mixture and was heated to 200° C. for 3 h and then at 120° C. overnight under nitrogen. The cooled reaction mixture was diluted with ethyl acetate and water. The mixture was filtered through Celite® and the Celite® was washed with ethyl acetate and water. The layers were separated and the aqueous layer was extracted with ethyl acetate. The organic layers were washed with brine, dried over magnesium sulfate, filtered, and evaporated. The residue was purified by column chromatography eluting with ethyl acetate to give pure product (2.4 g, 43%).

1. customNitrogen was bubbled directly into the mixture
2. customat 120° C.
3. customovernight
4. customThe cooled reaction mixture
5. filtrationThe mixture was filtered through Celite®
6. washthe Celite® was washed with ethyl acetate and water
7. customThe layers were separated
8. extractionthe aqueous layer was extracted with ethyl acetate
9. washThe organic layers were washed with brine
10. dry with materialdried over magnesium sulfate
11. filtrationfiltered
12. customevaporated
13. customThe residue was purified by column chromatography
14. washeluting with ethyl acetate