反应详情

Add 4-chlorobutyrophenone (50 g, 274 mmol), ethylene glycol (28 g, 452 mmol) and p-toluenesulfonic acid (1.04 g, 5.48 mmol) to benzene (600 mL) and heat at reflux for 16 h under a water trap. Cool the reaction to RT and wash with 1 N NaOH (500 mL) and brine (750 mL). Dry (sodium sulfate) and concentrate to give a solid. Recrystallize the solid from hot hexanes to give the title compound as a white powder (38 g, 61%).

1. temperatureheat
2. temperatureat reflux for 16 h under a water trap
3. temperatureCool
4. customthe reaction to RT
5. washwash with 1 N NaOH (500 mL) and brine (750 mL)
6. dry with materialDry (sodium sulfate)
7. concentrationconcentrate
8. customto give a solid
9. customRecrystallize the solid from hot hexanes