反应详情

120 mg (0.805 mmol) of 3-fluoro-4-formylbenzonitrile, 80.6 mg (0.805 mmol) of 2,4-pentanedione, 72.5 mg (1.21 mmol) of acetic acid and 14 mg (0.16 mmol) of piperidine are dissolved in 8 ml of dichloromethane and heated under reflux with an inverse water trap overnight. The mixture shows complete conversion (TLC check, mobile phase: cyclohexane/ethyl acetate 5:1). The mixture is diluted with dichloromethane, washed with water and saturated sodium chloride solution and dried with sodium sulfate. The solvent is removed in a rotary evaporator. 155 mg (83.3% of theory) of 4-(2-acetyl-3-oxobut-1-en-1-yl)-3-fluorobenzonitrile are obtained and are reacted without further purification.

1. temperatureheated
2. temperatureunder reflux with an inverse water trap overnight
3. washwashed with water and saturated sodium chloride solution
4. dry with materialdried with sodium sulfate
5. customThe solvent is removed in a rotary evaporator