摘要
[目的]改进丁噻隆的合成技术。[方法]用氢氧化钠溶液取代硫磺,高收率合成了N-甲基氨基硫脲,该步收率为73.8%;N-甲基氨基硫脲与特戊酰氯、三氯氧磷环合得2-甲基氨基-5-叔丁基-1,3,4-噻二唑,不使用浓硫酸作催化剂,反应后体系不需处理;2-甲基氨基-5-叔丁基-1,3,4-噻二唑在酰基化催化剂作用下与N-甲基甲酰氯合成丁噻隆,催化剂用量少,成本低,反应收率为95%;用甲苯作溶剂,整个反应过程简单、高效。[结果]合成路线3步总收率70.1%。[结论]该工艺简单经济,适合工业化生产。
[Aims] Synthesis technology of tebuthiuron was improved. [Methods] Using sodium hydroxide instead of sulfur to synthesize 4-methyl-thiosemicarbazide with high yield, the yield was 73.8%; 4-methyl-thiosemicarbazide, phosphorus oxychloride and trimethylacetyl chloride were reacted to get 2-methylamino-5-t-butyl-l,3,4-triadiazole, sulfuric acid was not used, product was not separated from solvent after the reaction; 2-methylamino-5-t-butyl-l,3,4-triadiazole and N-methylcarbamyl chloride were reacted catalyzed by DMAP to get tebuthiuron with yield of 95%; the whole process of the reactions was simple and efficient with toluene as solvent. [Results] The total yield was 70.1% based on methyl amine. [Conclusions] This process is simple and economical, which is suitable for industrial scale manufacture.
出处
《农药》
CAS
北大核心
2012年第10期715-716,共2页
Agrochemicals
关键词
丁噻隆
除草剂
合成
tebuthiuron
herbicide
synthesis
