反应详情

4-Trifluoromethylbenzaldehyde (25.0 mL, 147 mmol, 1.00 equiv), 2,2-dimethyl-1,3-dioxane-4,6-dione (21.2 g, 147 mmol, 1.00 equiv), methyl acetoacetate (15.8 mL, 147 mmol, 1.00 equiv), and ammonium acetate (11.8 g, 154 mmol, 1.05 equiv) were dissolved in acetic acid (150 mL) and heated to reflux for 2 hours. Addition of water to the stirred reaction mixture induced precipitation of a solid residue. The solid was recovered by filtration and triturated with 50% CH2Cl2/hexane to afford 8.50 g (19%) of the product as a white solid. MS (ES+) m/e 300 [M+H]+.

1. temperatureheated
2. temperatureto reflux for 2 hours
3. customto the stirred reaction mixture
4. customprecipitation of a solid residue
5. filtrationThe solid was recovered by filtration
6. customtriturated with 50% CH2Cl2/hexane