反应详情

N-(4-Amino-2-benzyloxy-phenyl)-4-fluoro-2-hydroxy-benzamide (76) (0.060 g, 0.170 mmol) was dissolved in THF (3.4 mL), NaHCO3 (0.086 g, 1.02 mmol) was added and the mixture was chilled on a dry-ice/acetone bath. Cyanuric chloride (5) (0.032 g, 0.184 mmol) was dissolved in THF (2 mL) and added directly to the chilled solution while stirring. The ice bath was removed and the mixture continued to stir while warming to room temperature for 1 h. TLC (Rf: 0.8 compared to Rf: 0.35 for compound 76 in 1:1 hexane/EtOAc, single spot) indicated complete reaction at this point. The reaction mixture was used immediately in the next step without purification or characterization.

1. temperaturethe mixture was chilled on a dry-ice/acetone bath
2. additionadded directly to the chilled solution
3. customThe ice bath was removed
4. stirringto stir
5. customreaction at this point
6. customThe reaction mixture was used immediately in the next step without purification or characterization