反应详情

温度

0 °C

To a stirred solution of 2-(Trifluoromethoxy)benzylamine (58.6 mg, 0.307 mmol) in toluene (1.239 mL) at 0° C. was added trimethylaluminium (2M in toluene, 0.557 mL, 1.115 mmol) dropwise. The mixture was stirred for 5 min at 0° C., then a solution of 95 (125 mg, 0.279 mmol) in toluene (0.620 mL) was added dropwise. The mixture was stirred at room temperature for 1 h, then at 55° C. for 1 h, and at 95° C. for 1.5 h till the reaction was complete. Saturated NaHCO3 was added to the reaction mixture followed by extraction with EtOAc. The organic extracts were dried over MgSO4, filtrated and concentrated and the residue was purified via Biotage (5% to 20% MeOH/CH2Cl2; 12M column) to give 99 as yellow oil. LRMS (ESI): calc.593.6; found 594.3 (MH)+.

1. stirringThe mixture was stirred at room temperature for 1 h
2. waitat 55° C. for 1 h
3. waitat 95° C. for 1.5 h till the reaction was complete
4. extractionfollowed by extraction with EtOAc
5. dry with materialThe organic extracts were dried over MgSO4
6. filtrationfiltrated
7. concentrationconcentrated
8. customthe residue was purified via Biotage (5% to 20% MeOH/CH2Cl2; 12M column)