反应详情

温度

120 °C

A mixture of 3-chloro-2-fluoro-aniline (10.9 g, 75 mmol) and 4-chloro-benzaldehyde (10.0 g, 71 mmol) was heated to 120° C., stirred for 18 h, allowed to cool to rt, and diluted with toluene (50 mL). A mixture of the sodium salt of 5-methyl-2,4-dioxo-hexanoic acid ethyl ester (14.8 g, 71 mmol) in dioxane (50 mL) and acetic acid (4.1 mL, 71 mmol) was added. The resulting mixture was refluxed for 18 h, allowed to cool to rt, diluted with EtOAc, and washed twice with an aqueous solution of NaHCO3 and brine. The crude product, obtained after drying and concentration, was triturated with EtOAc/hexane to provide 14 g of the title compound. tR: 5.23 min (HPLC 1); ESI-MS: 408 [M+H]+ (LC-MS1).

1. temperatureto cool to rt
2. additionwas added
3. temperatureThe resulting mixture was refluxed for 18 h
4. temperatureto cool to rt
5. washwashed twice with an aqueous solution of NaHCO3 and brine
6. customThe crude product, obtained
7. customafter drying
8. concentrationconcentration
9. customwas triturated with EtOAc/hexane