反应详情

Malonic acid (7.29 g, 70.0 mmol), 4-chlorobenzaldehye (9.84 g, 70.0 mmol) and ammonium acetate (10.9 g, 140 mmol) were heated in ethanol (15 ml) at 55° C. for 15 hours. Upon cooling the solvent was removed under reduced pressure and the residue was suspended in water and basified to pH 8 using saturated sodium carbonate solution. The aqueous was extracted with dichloromethane (3×) and the combined organic extracts were washed with brine, dried (MgSO4), filtered and evaporated under reduced pressure to afford the title compound as a cream solid, 3.48 g.

1. temperatureUpon cooling the solvent
2. customwas removed under reduced pressure
3. extractionThe aqueous was extracted with dichloromethane (3×)
4. washthe combined organic extracts were washed with brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated under reduced pressure