反应详情

温度

100 °C

A mixture of Compound 10 (1.25 g, 2.43 mmol), 9-(4′-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-[1,1′-biphenyl]-4-yl)-9H-carbazole (1.123 g, 2.52 mmol), tetrakis(triphenylphosphine) palladium(0) (0.14 g, 0.12 mmol), potassium carbonate (1.00 g, 7.27 mmol), 1,4-dioxane (25.00 mL), and water (5.00 mL) was degassed with bubbling argon for 45 minutes at 50° C. The reaction was then heated to 100° C. and stirred overnight (17 hours), maintaining an argon atmosphere. The precipitated product was filtered (filtrate saved for later purification), dried, and purified by column chromatography, on a silica gel column, with acetone in hexanes as the eluent. The product fractions were then dried to yield Host-4 (1.09 g). On the filtrate from the initial filtration, the material was extracted with ethyl acetate, dried, and purified by column chromatography, with the same eluent as the first column. The product fractions were then dried and combined with the collected product from the first column to yield a total of 1.40 g (76.2%) of Host-4. Confirmed by LCMS (APCI): calculated for C55H35N3O (M+H): 754. Found: 754.

1. customwas degassed with bubbling argon for 45 minutes at 50° C
2. temperaturemaintaining an argon atmosphere
3. filtrationThe precipitated product was filtered
4. custom(filtrate saved for later purification)
5. customdried
6. custompurified by column chromatography, on a silica gel column, with acetone in hexanes as the eluent
7. customThe product fractions were then dried
8. customto yield Host-4 (1.09 g)
9. filtrationOn the filtrate from the initial filtration
10. extractionthe material was extracted with ethyl acetate
11. customdried
12. custompurified by column chromatography, with the same eluent as the first column
13. customThe product fractions were then dried
14. customto yield a total of 1.40 g (76.2%) of Host-4