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乙嘧硫磷合成工艺研究
Study on the Synthesis of Etrimfos
【摘要】 通过单因子实验考察了影响乙嘧硫磷收率的因素,得出了合成乙嘧硫磷的较佳工艺条件:以乙酸乙酯为溶剂、氢氧化钠为缚酸剂、4-二甲氨基吡啶为催化剂,其用量为原料2-乙基-4-乙氧基-6-羟基嘧啶的4%(摩尔比)、物料配比n(2-乙基-4-乙氧基-6-羟基嘧啶)∶n(氢氧化钠)∶n(O,O-二甲基硫化磷酰氯)=1∶1.2∶1.1、反应温度为45°C,反应时间为5 h。产品收率为91%,含量为74.0%。用液相色谱-质谱、红外光谱、核磁共振谱对产品结构进行了分析,证明所得产物为目标产物。
【Abstract】 The influential factors of synthesizing etrimfos were investigated by single factor experiments.The optimum reaction conditions were as follows: ethyl acetate as solvent;sodium hydroxide solid as acid-receptor;4-dimethylaminopyridine as phase transfer catalyst;its amount was 4% of the amount of 2-ethyl-4-ethoxy-6-hydroxypyrimidine;molar ratio of 2-ethyl-4-ethyoxy-6-hydroxypyrimidine∶sodium hydroxide∶O,O-dimethyl thiophospyhoryl chloride=1∶1.2∶1.1;reaction temperature was 45°C;reaction time was 5 h.The yield of etrimfos was 91%,with the purity of 74%.The product was identified by LC-MS,IR,()~1H NMR.
- 【文献出处】 化学世界 ,Chemical World , 编辑部邮箱 ,2008年01期
- 【分类号】TQ453
- 【被引频次】2
- 【下载频次】188