摘要
3-甲基-7-硝基苯酞是嘧啶水杨酸类除草剂环酯草醚的一个重要中间体,以3-硝基邻苯二甲酸、乙酸酐和丙二酸二乙酯为原料,经脱水缩合、Knoevenagel反应、水解脱羧及硼氢化钠还原合成.考察了各步反应溶剂、反应温度、反应时间和原料配比等因素对反应收率的影响.在最佳优化反应条件下,反应总收率为57.8%,产品质量分数为98.8%,其结构经红外IR和氢谱核磁1 H NMR分析确证.该工艺路线简单、经济、合理并适合于工业化生产.
3-methyl-7-nitrophthalide was regarded as an important intermediate for the pyriftalid of pyrimidylsalicylate herbicides, using 3-nitrophthalic acid, acetic anhydride and diethyl malonate as raw materials, 3-methyl-7-nitrophthalide was prepared through the successive reactions of dehydration-condensation, Knoevenagel, hydrolysis decarboxylation and borohydride reduction. We investigate the effect of the reaction solvent, reaction temperature, reaction time and the ratio of raw materials and other factors for each step on the yield Under the optimized conditions of reactions, the total yield of 3-methyl-7-nitrophthalide was 57. 8%, the purity was 98. 8%. The structures of the product and the intermediate were confirmed by IR and 1 H NMR. This new technology is simple, reasonable and economical, so that it is very suitable for industrial production.
出处
《浙江工业大学学报》
CAS
2013年第2期195-198,共4页
Journal of Zhejiang University of Technology
作者简介
苗丽（1986-），女，山西忻州人，硕士研究生，研究方向为农药合成及剂型研究，E—mail：miaolil7@163．com．
通信作者：来虎钦教授，E-mail：laihuq@tom．com．
