6-氯-3-甲基嘧啶-4(3H)-酮的合成及表征
Synthesis and characterization of 6-chloro-3-methylpyrimidin-4(3H)-one
韩磊 1李晓花 1党小琳 1唐文强 1杜漠1
作者信息
- 1. 咸阳市分子影像与药物合成重点实验室,陕西国际商贸学院医药学院,陕西咸阳 712046
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摘要
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).
Abstract
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).
关键词
嘧啶衍生物/N-甲基化反应/结构表征/合成Key words
pyrimidine derivatives/N-methylation reaction/structure characterization/synthesis引用本文复制引用
出版年
2025
NETL
NSTL
万方数据