反应详情

To a stirred solution of 1-amino-1H-1,2,4-triazole (75% purity, 5.6 g, 0.05 mmol) and 2-(4-chlorophenoxy)-4'-fluoroacetophenone (13.2 g, 0.05 mmol) in 100 mL dry toluene is added a catalytic amount (1.0 g) p-toluene sulfonic acid. The mixture is heated at reflux with azeotropic removal of water for 4 days. Solvent is evaporated and the residue taken up in 200 mL ethyl acetate. The organic solution is washed with 2×100 mL 10% aqueous Na2CO3 and 1×100 mL brine. The dried (MgSO4) solution is filtered and concentrated to give the desired product which can be purified by chromatography or crystallization from an appropriate solvent.

1. temperatureThe mixture is heated
2. customSolvent is evaporated
3. washThe organic solution is washed with 2×100 mL 10% aqueous Na2CO3 and 1×100 mL brine
4. dry with materialThe dried (MgSO4) solution
5. filtrationis filtered
6. concentrationconcentrated