反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
3.8 g (0.0373 mol) of triethylamine were added at -20° C. to a mixture of 5 g (0.0373 mol) of 2,4,6-trifluoropyrimidine in 50 ml of methanol within 5 minutes, and the mixture was stirred at this temperature for a further 40 minutes. After the reaction was complete, the mixture was warmed to 25° C. and the excess methanol was removed by distillation under reduced pressure. The residue obtained in this way was partitioned between methylene chloride and water, and the organic phase was dried over magnesium sulfate and concentrated. 4.6 g (85% of theory) of an isomer mixture which, according to investigation by gas chromatography, contained 46% of the title compound and 48% of 4,6-difluoro-2-methoxypyrimidine were obtained in this way.
WORKUP
后处理
- customthe excess methanol was removed by distillation under reduced pressure
- customThe residue obtained in this way
- customwas partitioned between methylene chloride and water
- dry with materialthe organic phase was dried over magnesium sulfate
- concentrationconcentrated