反应详情

温度

40 °C

To a 100 L cylindrical vessel with heating coils were charged EtOAc (20 L) and TsOH/H2O (2.304 kg, 12.11 mol), and the mixture was heated to 35-45° C. to dissolve. The acid solution was fed into the isoxazole batch with further distilling, maintaining a constant volume of 25 L. An additional 20 L of EtOAc was distilled to azeotropically dry the mixture. A slurry began to form, and it continued to thicken on addition and concentration. The final KF was 400 ppm water. The batch was heated to 60° C. and allowed to slowly cool to ambient temperature overnight.

1. dissolutionto dissolve
2. temperaturemaintaining a constant volume of 25 L
3. distillationAn additional 20 L of EtOAc was distilled
4. customto azeotropically dry the mixture
5. customto form
6. additionto thicken on addition and concentration
7. temperatureThe batch was heated to 60° C.
8. temperatureto slowly cool to ambient temperature overnight