反应详情

A suspension of (R)-3-bromo-4-(3-hydroxypyrrolidin-1-yl)-N-(4-(trifluoromethoxy)phenyl)benzamide (Stage 1.2, 100 mg, 0.225 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazole (146 mg, 0.45 mmol), Pd(PPh3)2Cl2 (17.34 mg, 0.025 mmol) and Na2CO3 (119 mg, 1.123 mmol) in a mixture of water (272 μL), DME (953 μL) and EtOH (136 μL) was subjected to MW irradiation at 125° C. for 20 min. The RM was diluted with THF (3 mL), treated with Si-Thiol (Silicycle, 1.44 mmol/g, 94 mg, 0.135 mmol), filtered and the filtrate was evaporated off under reduced pressure to give a residue which was purified by flash chromatography (RediSep® Silica gel column, 4 g, cyclohexane/EtOAc from 40% to 100% EtOAc) to yield the title compound as a yellow oil. UPLC-MS (Condition 1) tR=3.28 min, m/z=563.2 [M+H]+, m/z=561.2 [M−H]−.

1. customwas subjected to MW irradiation at 125° C. for 20 min
2. filtrationfiltered
3. customthe filtrate was evaporated off under reduced pressure
4. customto give a residue which
5. customwas purified by flash chromatography (RediSep® Silica gel column, 4 g, cyclohexane/EtOAc from 40% to 100% EtOAc)