以6-氯嘧啶-4(3H)-酮和碘甲烷为原料,经N-甲基化反应得到产物6-氯-3-甲基嘧啶-4(3H)-酮.产物结构经1 HNMR、13CNMR、1 H-1 H NOESY和ESI-MS表征.优化并确定N-甲基化反应的适宜条件为:N,N-二甲基甲酰胺为溶剂、物料比n(碘甲烷)∶n(6-氯嘧啶-4(3H)-酮)=1.5∶1、反应温度60℃、反应时间12h.在该条件下,产物的收率达到78.8％(以6-氯嘧啶-4(3H)-酮计).
Synthesis and characterization of 6-chloro-3-methylpyrimidin-4(3H)-one
The product of 6-chloro-3-methylpyrimidin-4(3H)-one was obtained through N-methylation reaction of 6-chloro-pyrimidin-4(3H)-one and methyl iodide as raw materials.The structure of the product was characterized by 1HNMR,13CNMR,1H-1H NOESY and ESI-MS.The optimized suitable conditions for the N-methylation reaction were determined as follows:N,N-dimethylformamide as the solvent,material ratio of n(methyl iodide)∶n(6-chloro-pyrimidin-4(3H)-one)=1.5∶1,reaction temperature was 60℃,and reaction time was 12h.Under these conditions,the yield of the product reached 78.8％(based on 6-chloro-pyrimidin-4(3H)-one).
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