反应详情

温度

100 °C

A mixture of Compound 10 (1.25 g, 2.43 mmol), Compound 11 (0.931 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, dried, purified by silica gel column chromatography with acetone in hexanes as the eluent, and recrystallized from acetone/hexanes. The recrystallized product was collected to yield Host-5 (1.34 g, 82%). Confirmed by LCMS (APCI): calculated for C49H31N3O (M+H): 678. Found: 678.

1. customwas degassed with bubbling argon for 45 minutes at 50° C
2. temperaturemaintaining an argon atmosphere
3. filtrationThe precipitated product was filtered
4. customdried
5. custompurified by silica gel column chromatography with acetone in hexanes as the eluent
6. customrecrystallized from acetone/hexanes
7. customThe recrystallized product was collected
8. customto yield Host-5 (1.34 g, 82%)