反应详情

A mixture of 8.9 g (36.2 mmole) 3-bromo-9H-carbazole, 10.6 g (36.2 mmole) of 2-iododibenzo[b,d]furan, 17.1 g (90 mmole) of copper(I) iodide, 19.1 g (90 mmole) of potassium phosphate, 10.3 g (90 mmole) of trans-1,2-cyclohexanediamine and 1,4-dioxane 700 ml were refluxed under nitrogen for about overnight. Then, the solution was filtered at 110° C. To receive the filtrate, And the 1,4-dioxane was removed under reduced pressure from the filtrate. The filtrate was extracted with 500 ml dichloromethane and 2000 ml water, the organic layer was dried with anhydrous magnesium sulfate, the solvent was removed and the residue was purified by column chromatography on silica (hexane-ethyl acetate) to give product 8.4 g (56%).

1. temperaturewere refluxed under nitrogen for about overnight
2. filtrationThen, the solution was filtered at 110° C
3. customthe 1,4-dioxane was removed under reduced pressure from the filtrate
4. extractionThe filtrate was extracted with 500 ml dichloromethane and 2000 ml water
5. dry with materialthe organic layer was dried with anhydrous magnesium sulfate
6. customthe solvent was removed
7. customthe residue was purified by column chromatography on silica (hexane-ethyl acetate)