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Yield and Purity Comparison of Dimethoate Manufacturing Processes: Homogeneous Reaction, Two-Phase Uncatalyzed Reaction, and Phase Transfer Catalysis

机译:乐果生产工艺的收率和纯度比较:均相反应,两相未催化反应和相转移催化

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摘要

The process for manufacturing dimethoate (O,O-dimethyl S-methylcarbamoylmethyl phosphoro-dithioate) should provide high yields of highly pure product which requires no further purification steps. A comparison of dimethoate yield and purity obtained by different manufacturing processes is presented. Ethanol, isopropanol, acetone, ethyl methyl ketone, and isobutyl methyl ketone were the solvents used when the reaction was carried out in one single homogeneous phase. In heterogeneous aqueous—organic solvent medium, an analysis by linear regression techniques has revealed temperature, reaction time, and organic solvent volume as the operational variables with statistical significance above 95% on the dimethoate purity, while only temperature was significant on gross and net yields. The phase transfer catalysis did not improve purity and yield obtained in heterogeneous solvent medium with any of the studied catalysts, namely methyltrioctylammonium chloride, tetrabutylammonium bromide, tetraoctyl-ammonium bromide, tetraphenylphosphonium bromide, and tetrabutylphosphonium bromide.
机译:制造乐果的方法(O,O-二甲基S-甲基氨基甲酰基甲基二硫代磷酸酯)应提供高收率的高纯产物,无需进一步纯化步骤。比较了通过不同制造工艺获得的乐果的收率和纯度。当在一个单一的均相中进行反应时,使用的溶剂有乙醇,异丙醇,丙酮,乙基甲基酮和异丁基甲基酮。在非均质的水性有机溶剂介质中,通过线性回归技术进行的分析表明,温度,反应时间和有机溶剂体积是操作变量,对乐果纯度的统计显着性高于95%,而只有温度对总收率和净产率有显着影响。使用任何已研究的催化剂,即甲基三辛基氯化铵,溴化四丁基铵,溴化四辛基铵,溴化四苯基phosph和溴化四丁基phosph,相转移催化均不能提高在多相溶剂介质中获得的纯度和收率。

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