反应详情

温度

140 °C

DIPEA (0.115 mL, 0.660 mmol) was added to a solution of 5-bromo-6-chloro-N-(4-(trifluoromethoxy)phenyl)nicotinamide (Stage 6.2, 119 mg, 0.3 mmol) and azetidin-3-yl-methanol, HCl salt (44.5 mg, 0.36 mmol) in iPrOH (0.3 mL) in a vial, which was sealed and the RM mixture stirred at 140° C. for 5 h. After cooling at RT, the RM was dissolved in EtOAc, washed with 0.5 M HCl and brine, dried over Na2SO4 and the solvent was evaporated off under reduced pressure to give a crude product which was purified by flash chromatography (Silica gel column, n-hexane/EtOAc from 50% to 100% EtOAc) and crystallized from n-pentane/EtOAc to afford the title product as white crystals. HPLC (Condition 4) tR=5.33 min, UPLC-MS (Condition 3) tR=1.06 min, m/z=446.2 [M+H]+.

1. customwas sealed
2. temperatureAfter cooling at RT
3. washwashed with 0.5 M HCl and brine
4. dry with materialdried over Na2SO4
5. customthe solvent was evaporated off under reduced pressure
6. customto give a crude product which
7. customwas purified by flash chromatography (Silica gel column, n-hexane/EtOAc from 50% to 100% EtOAc)
8. customcrystallized from n-pentane/EtOAc