反应详情

温度

140 °C

5-Bromo-6-chloro-N-(4-((trifluoromethyl)thio)phenyl)nicotinamide (Stage 185.2, 206 mg, 0.5 mmol) and (S)-pyrrolidin-3-ol (52.3 mg, 0.6 mmol) were dissolved in iPrOH (0.5 mL). DIPEA (192 μL, 1.1 mmol) was added and the RM mixture was heated at 140° C. for 1 h in a pressure safe vial. The vial was cooled to RT and the RM was evaporated to dryness under reduced pressure to give residue that was purified by flash chromatography (RediSep® Silica gel column, n-heptane/EtOAc, from 20% to 100% EtOAc). Trituration with n-heptane, filtered and dried afforded the title compound as a white crystalline powder. HPLC (Condition 4) tR=5.89 min, UPLC-MS (Condition 3) tR=1.20 min, m/z=464.1 [M+H]+.

1. temperatureThe vial was cooled to RT
2. customthe RM was evaporated to dryness under reduced pressure
3. customto give residue that
4. customwas purified by flash chromatography (RediSep® Silica gel column, n-heptane/EtOAc, from 20% to 100% EtOAc)
5. filtrationTrituration with n-heptane, filtered
6. customdried