反应详情

A mixture of DME (570 μL), water (163 μL) and EtOH (81 μL) was added to a mixture of (R)-5-bromo-6-(3-hydroxypyrrolidin-1-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide (Stage 2.2, 60 mg, 0.134 mmol), (1H-pyrazol-3-yl)boronic acid (45.1 mg, 0.403 mmol) Pd(PPh3)2Cl2 (9.44 mg, 0.013 mmol), Na2CO3 (42.8 mg, 0.403 mmol) in a MW vial. The vial was sealed, evacuated/purged 3 times with argon and the RM was subjected to MW irradiation at 120° C. for 10 min. Additional (1H-pyrazol-3-yl)boronic acid (45.1 mg, 0.403 mmol) was added and the RM was subjected to MW irradiation at 120° C. for 30 min, diluted with THF (1 mL) and treated with Si-Thiol (Silicycle 1.27 mmol/g, 52.9 mg, 0.067 mmol), filtered and the filtrate was evaporated off under reduced pressure to give a residue which was purified by preparative HPLC (Condition 9, 15% for 0.2 min then 15% to 45% in 14 min) to yield the title compound as a white solid.

1. customThe vial was sealed
2. customevacuated/purged 3 times with argon
3. customthe RM was subjected to MW irradiation at 120° C. for 10 min
4. customthe RM was subjected to MW irradiation at 120° C. for 30 min
5. filtrationfiltered
6. customthe filtrate was evaporated off under reduced pressure
7. customto give a residue which
8. customwas purified by preparative HPLC (Condition 9, 15% for 0.2 min