反应详情

A mixture of 3-bromo-N-(4-(trifluoromethoxy)phenyl)benzamide (Stage 3.1, 50 mg, 0.139 mmol in 2.4 mL DME), methyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)thiophene-2-carboxylate (0.180 mmol), 2 M Na2CO3 (0.104 mL, 0.208 mmol), water (0.8 mL), and (Ph3P)4Pd (8 mg, 6.94 μmol) in a sealed vial were subjected to MW irradiation at 150° C. for 10 min. The RM was filtered through a PL-Thiol MP SPE cartridge (StratoSpheres™, 6 mL), the cartridge was washed with MeOH (10 mL) and the combined filtrates were evaporated to dryness under reduced pressure to give the crude product was purified by preparative HPLC to afford the title compound. UPLC-MS (Condition 6) tR=2.37 min, m/z=422.3 [M+H]+.

1. customvial were subjected to MW irradiation at 150° C. for 10 min
2. filtrationThe RM was filtered through a PL-Thiol MP SPE cartridge (StratoSpheres™, 6 mL)
3. washthe cartridge was washed with MeOH (10 mL)
4. customthe combined filtrates were evaporated to dryness under reduced pressure
5. customto give the crude product
6. customwas purified by preparative HPLC