反应详情

Dissolve trifluoromethanesulfonic acid 1-[4-(2-azepan-1-yl-ethoxy)-benzoyl]-6-methoxynaphthalen-2-yl ester (1.68 g, 3.05 mmol) in 30 mL of acetonitrile and add 2-fluorobenzene boronic acid (0.85 g, 6.10 mmol), trans[dichlorobis(triphenylphosphine)]palladium II (0.43 g, 0.61 mmol) and sonicate briefly. Next add cesium fluoride (4.17 g, 27.45 mmol) and heat to 75° C. for 1 hour. Add Celite and filter. Concentrate the solvent under vacuum, dissolve in methanol and purify on an SCX cartridge, eluting with 2 N ammonia/methanol. Purify further on a silica gel column eluting with a 0-10% methanol/methylene chloride gradient to isolate 1.10 g of the title compound (72%).

1. customsonicate briefly
2. filtrationAdd Celite and filter
3. concentrationConcentrate the solvent under vacuum
4. dissolutiondissolve in methanol
5. custompurify on an SCX cartridge
6. washeluting with 2 N ammonia/methanol
7. customPurify further on a silica gel column
8. washeluting with a 0-10% methanol/methylene chloride gradient