反应详情

A mixture of 5-bromo-6-((3-hydroxypropyl)amino)-N-(4-(trifluoromethoxy)phenyl)nicotinamide (Stage 161.1, 72 mg, 0.15 mmol), pyrimidin-5-ylboronic acid (18.7 mg, 0.15 mmol) and Na2CO3 (48 mg, 0.450 mmol) in a mixture of DME (3.2 mL), EtOH (0.43 mL) and water (0.64 mL) was flushed with argon for 5 min. Pd(PPh3)2Cl2 was added (5.3 mg, 0.0075 mmol) and the mixture was subjected to MW irradiation at 125° C. for 20 min. The vial was cooled to RT and the RM was evaporated to dryness under reduced pressure to give a residue that was triturated with THF and filtered. The filtrate was evaporated to dryness under reduced pressure and the crude product was purified by preparative LC-MS. TFA was removed using a SPE PL-HCO3 (StratoSpheres™ VariPure IPE) cartridge to afford the title compound. UPLC-MS (Condition 8) tR=2.05 min, m/z=434.1 [M+H]+, m/z=432.1 [M−H]−.

1. customwas flushed with argon for 5 min
2. additionPd(PPh3)2Cl2 was added (5.3 mg, 0.0075 mmol)
3. customthe mixture was subjected to MW irradiation at 125° C. for 20 min
4. customthe RM was evaporated to dryness under reduced pressure
5. customto give a residue that
6. customwas triturated with THF
7. filtrationfiltered
8. customThe filtrate was evaporated to dryness under reduced pressure
9. customthe crude product was purified by preparative LC-MS
10. customTFA was removed