反应详情

温度

120 °C

A mixture of 5-bromo-6-chloro-N-(4-(1,1-difluoroethoxy)phenyl)nicotinamide (Stage 30.2, 700 mg, 1.752 mmol), (R)-pyrrolidin-3-ol (0.170 mL, 2.102 mmol) and DIPEA (0.673 mL, 3.85 mmol) and iPrOH (2 mL) in a sealed vial was heated to 120° C. for 1 h. The RM was diluted with EtOAc (80 mL), treated with citric acid 10% (40 mL; ˜pH4) and extracted with EtOAc. The combined extracts were washed with brine (2×40 mL), dried over Na2SO4 and the solvent was evaporated off under reduced pressure to give a residue which was washed with Et2O and n-hexane and the crystals were dried to give the title product as a beige solid. HPLC (Condition 5) tR=6.4 min, UPLC-MS (Condition 3) tR=1.02 min, m/z=442.1/444.0 [M+H]+.

1. extractionextracted with EtOAc
2. washThe combined extracts were washed with brine (2×40 mL)
3. dry with materialdried over Na2SO4
4. customthe solvent was evaporated off under reduced pressure
5. customto give a residue which
6. washwas washed with Et2O and n-hexane
7. customthe crystals were dried