反应详情

A mixture of 1,1-dimethylethyl 4-[(6-bromo-1,2-benzisoxazol-3-yl)acetyl]-1-piperazinecarboxylate (Intermediate 33) (0.045 g) N-cyclopropyl-4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (Intermediate 5) (0.03 g) and 2M aqueous sodium carbonate (0.65 ml) in isopropanol (2.5 ml) under nitrogen was treated with tetrakis(triphenylphosphine)palladium(0) (1 mg) then stirred at reflux for 18 h. On cooling the mixture was absorbed onto silica (Merck 7734) and applied to a Varian Bond-Elut SPE cartridge (silica, 5 g). Sequential elution with dichloromethane, chloroform, ether, ethyl acetate, acetonitrile and acetone yielded the title compound as a white solid (0.03 g).

1. temperatureat reflux for 18 h
2. temperatureOn cooling the mixture
3. customwas absorbed onto silica (Merck 7734)
4. washSequential elution with dichloromethane, chloroform, ether, ethyl acetate, acetonitrile and acetone