摘要
以嘧啶醇和碳酸钾水溶液在有机溶剂中反应减压脱水,生成嘧啶醇钾盐与甲基氯化物进行缩合反应,经过滤、减压浓缩得到甲基嘧啶磷。优化的反应条件为:以甲苯为溶剂,n(嘧啶醇)∶n(碳酸钾)=1.0∶2.0,嘧啶醇钾盐含水量<0.1%,反应温度30~40℃,反应时间6 h。优化条件下,甲基嘧啶磷纯度98.5%,收率92.6%,该工艺转化率高、收率高、三废少,符合绿色环保生产理念,具有工业化应用前景。
Pyrimidine alcohol and potassium carbonate aqueous solution were reacted in organic solvent to dehydrate under reduced pressure,resulting in the condensation reaction of pyrimidinol potassium salt with methyl chloride,and methyl pyrimidinophos was obtained by filtration and concentration under reduced pressure.The optimised conditions were as follows:toluene as solvent,n(pyrimidinol)∶n(potassium carbonate)=1.0∶2.0,water content of pyrimidinol potassium salt<0.1%,reaction temperature 30~40℃,reaction time 6 h.The content of the product under the optimised conditions was 98.5%and the yield was 92.6%.The process has high conversion rate,high yield and less waste.In line with green environmental protection production concept,it has the prospect of industrial production.
作者
竺来发
尤瑶瑶
张海涛
干兴利
张秋影
刘双瑾
李艳琼
ZHU Lai-fa;YOU Yao-yao;ZHANG Hai-tao;GAN Xing-li;ZHANG Qiu-ying;LIU Shuang-jin;LI Yanqiong(National Engineering Research Center for Agrochemicals,Hunan Research Institute of Chemical Industry Co.,Ltd.,Changsha 410014,China;Agrochemical Key Laboratory of Hunan Province,Changsha 410014,China;Hunan Haili Changde Pesticide Chemical Co.,Ltd.,Changde 415000,China)
出处
《精细化工中间体》
CAS
2024年第1期14-16,共3页
Fine Chemical Intermediates
基金
湖南省企业科技创新创业团队项目(湖南海利新材料科技创新创业团队)。
关键词
嘧啶醇
甲基嘧啶磷
碳酸钾
绿色合成
pyrimidine alcohol
pirimiphos-methyl
potassium carbonate
green synthesis