反应详情

温度

80 °C

85.0 g (0.5 mol) of 4-hydroxy-5-methoxy-6-methoxymethylpyrimidine were suspended in 600 ml of dichloroethane, 50.5 g of triethylamine were added, and 260 g (1.7 mol) of phosphorus oxychloride were then added without cooling. The mixture was stirred for 3 hours at 80° C., poured into ice-water and neutralized by adding solid sodium carbonate, the organic phase was separated, and the water phase was extracted several times by stirring with methylene chloride. The combined organic phases were dried and concentrated. The residue was distilled under a water pump vacuum. 66.1 g (70% of theory) of a yellow oil were obtained. B.p. 93°-96° C./0.1mm.

1. temperaturewithout cooling
2. customthe organic phase was separated
3. extractionthe water phase was extracted several times
4. stirringby stirring with methylene chloride
5. customThe combined organic phases were dried
6. concentrationconcentrated
7. distillationThe residue was distilled under a water pump vacuum
8. custom66.1 g (70% of theory) of a yellow oil were obtained