反应详情

3-Bromo-4-formyl-benzonitrile (intermediate 2, 3.25 g, 14.7 mmol) is stirred with acetylacetone (2.42 mL, 19.1 mmol), 3-(trifluoromethyl)phenylurea (3 g, 14.7 mmol) and polyphosphoric acid (3.02 g, 7.90 mmol) in tetrahydrofurane (80.0 mL) at 60° C. for 48 h. The reaction mixture is concentrated in vacuo and ethyl acetate and water is added and the phases are separated. The aqueous phase is extracted twice with ethyl acetate. The combined organic phases are washed with saturated sodium chloride solution, dried over MgSO4 and concentrated. Yield: 7.66 g; ESI mass spectrum: [M+H]+=508; Retention time HPLC: 1.14 min (HPLC method Z018_S04)

1. concentrationThe reaction mixture is concentrated in vacuo and ethyl acetate and water
2. additionis added
3. customthe phases are separated
4. extractionThe aqueous phase is extracted twice with ethyl acetate
5. washThe combined organic phases are washed with saturated sodium chloride solution
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. custom1.14 min (HPLC method Z018_S04)