反应详情

温度

245 °C

5-(((4-Bromo-3-fluorophenyl)amino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (61.14 g, 177.6 mmol) was added portion-wise to Dowtherm (270 mL) at 245° C. After the addition, stirred at 245° C. for 20 minutes. Cool to RT. Added hexanes (˜830 mL) and filtered the solid washing with additional hexanes and dried the solid to yield 6-bromo-7-fluoroquinolin-4(1H)-one/6-bromo-5-fluoroquinolin-4(1H)-one (38.02 g, 88.5%) as brown solid and as a mixture of regioisomers (46:54, by LCMS). MS: m/z: 242.0/244.0 [M+H]+. Used this mixture as is for the next step.

1. additionAfter the addition
2. temperatureCool to RT
3. filtrationAdded hexanes (˜830 mL) and filtered the solid
4. washwashing with additional hexanes
5. customdried the solid