反应详情

温度

70 °C

29.7 g (0.146 mol) of 4-hydroxy-5-bromo-6-ethylpyrimidine are introduced slowly into 27.3 g (0.178 mol) of phosphorus oxychloride. The suspension dissolves on heating to 70° C.; the reaction is slightly exothermic. The temperature is kept at 70° C. for 11/2 hours and, after cooling, the solution is poured onto ice-water and neutralised carefully to pH 5-7, at 0° C., with 30% sodium hydroxide solution. Extraction with ethyl acetate yields, after removal of the solvent, 30.4 g of crude product. Distillation yields 23.9 g (73.9% of the theoretical yield) of pure substance having a boiling point of 112°-114° C./24 mbar.

1. dissolutionThe suspension dissolves
2. customis kept at 70° C. for 11
3. custom2 hours
4. temperatureafter cooling
5. extractionExtraction with ethyl acetate
6. customyields
7. customafter removal of the solvent, 30.4 g of crude product
8. distillationDistillation
9. customyields 23.9 g (73.9% of the
10. customtheoretical yield) of pure substance