文献类型：期刊文献

中文题名：螺虫乙酯的合成

英文题名：Synthesis of Spirotetramat

作者：师文娟[1];廖道华[1];杨芳[1];刘少春[1];杜梦[1]

机构：[1]华东理工大学药学院,上海200237

年份：2010

卷号：49

期号：4

起止页码：250

中文期刊名：农药

外文期刊名：Agrochemicals

收录：CSTPCD;;北大核心:【北大核心2008】；

语种：中文

中文关键词：杀虫剂;螺虫乙酯;(4-甲氧基)-环己基-氨基甲酸甲酯;2,5-二甲基苯乙酰氯;合成

外文关键词：pestcide; spirotetramat; cis-4-methoxyl-cyclohexane-1-amino-carboxylic methyl ester; 2; 5-dimethylphenylacetyl chloride; synthesis

摘要：cis-8-甲氧基-1,3-二氮杂螺[4.5]癸-2,4-二酮水解得到含有cis-4-甲氧基环己基-1-氨基甲酸的混合物,对该混合物进行纯化处理得到cis-4-甲氧基环己基-1-氨基甲酸。cis-4-甲氧基环己基-1-氨基甲酸在饱和氯化氢的甲醇溶液中酯化,接着酰化,环合,最后与氯甲酸乙酯发生取代反应,生成目标产物螺虫乙酯。反应总收率72%,含量97.5%(HPLC,面积归一法),产物经1HNMR、MS进行了表征。
cis-8-Methoxy-1,3-diazaspiro[4.5]decane-2,4-dione was hydrolyzed to a mixture containing cis-4-methoxylcyclohexane-1-amino-carboxylic acid. The mixture was purified to obtain cis-4-methoxylcyclohexane-1-amino-carboxylic acid. cis-4-Methoxyl-cyclohexane-1-amino-carboxylic acid methyl ester was synthesized by esterification of cis-4-methoxylcyclohexane-1-amino-carboxylic acid in saturated solution of hydrogen chloride in methanol. Starting from cis-4-methoxylcyclohexane-1-amino-carboxylic acid methyl ester, spirotetramat was obtained via amidation, cyclization, substitution with ethyl chloroformate. The total yield of spirotetramat was 72%, and the content was 97.5%（HPLC）. The products were determined by 1H NMR and MS.