反应详情

温度

110 °C

2,4-Difluorobenzaldehyde (3.28 mL, 30 mmol), 2,2-dimethyl-1,3-dioxane-4,6-dione (4.32 g, 30 mmol), ammonium acetate (2.46 g, 32 mmol), and methyl 3-oxobutanoate (3.23 mL, 30 mmol) were combined in acetic acid (30 mL) under nitrogen. This mixture was heated to 110° C. for 1 h. The reaction mixture was cooled to room temperature and then poured into water (100 mL). The mixture was decanted to leave yellow oil and white solid, which was taken up in MeOH/EtOAc and then concentrated. The residue was triturated with 5% ether/hexanes to afford the title compound (2.72 g, 32%). MS (ES+) m/e 282 [M+H]+.

1. temperatureThe reaction mixture was cooled to room temperature
2. customThe mixture was decanted
3. customto leave yellow oil and white solid, which
4. concentrationconcentrated
5. customThe residue was triturated with 5% ether/hexanes