反应详情

A solution of benzyl propionylacetate (36.3 g, 176 mmol), 3,4-difluorobenzaldehyde (25.0 g, 176 mmol), piperidine (0.86 mL, 9.0 mmol) and acetic acid (0.49 mL, 9.0 mmol) was refluxed with removal of water using a Dean-Stark apparatus for 5 h. The solvent was removed in vacuo and the residue was dissolved in EtOAc. The reaction mixture was washed with water (100 mL), followed by brine (100 mL) and dried over anhydrous Na2SO4. The solvent was evaporated, giving a pale yellow syrup (60.2 g). The product was used in the next step without further purification.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was dissolved in EtOAc
3. washThe reaction mixture was washed with water (100 mL)
4. dry with materialdried over anhydrous Na2SO4
5. customThe solvent was evaporated