双胍辛醋酸盐杀菌剂及其两种中间体的合成与生物活性

Synthesis of fungicide bis-(8-guanidino-octyl)amine acetate and its intermediates and bioactivity

双胍辛醋酸盐是一种重要的农用和园艺用广谱型杀菌剂[1,2],以尿素、硫酸二甲酯及醋酸为主要原料,合成O-甲基异脲醋酸盐,其含量达到98%以上,总收率可达70%.以癸二酸、迭氮化钠及浓硫酸为主要原料,经两步工艺直接制得二亚辛基三胺,含量达到98%以上,总收率可达65%.利用FT-IR、1H NMR等技术表征它们的结构,并建立了有效的分析测试方法.以上述二中间体为主要原料合成了双胍辛醋酸盐杀菌剂,利用FT-IR、1HNMR等技术表征了其结构.生物活性测试结果表明,该杀菌剂为广谱型杀菌剂.合成路线如下.

O-methylisourea acetate was synthesized by two procedures from the main raw materials including carbamide,dimethyl sulfate,acetic acid and concentrated sulfuric acid.Its content reaches 98% and the total yield attains to 70%.1,17-Diamino-9-azaheptadecane was first synthesized by two procedures using sebcic acid,1,8-octanediamine,sodium azide and concentrated sulfuric acid as the main raw materials.Its content reaches 98% and the total yield is 65%.The structure of both were confirmed by FT—IR,()~1H NMR and their available analysis method was established.Fungicide bis-(8-guanidino-octy1)amine acetate was synthesized from these two intermediates and its structure was confirmed by FT—IR and ()~1HNMR.Fungicidal activity test showed that it is a kind of broad-spectrum fungicide with notably effect.