摘要
2-氟异丁酸甲酯作为农药中间体可以合成含氟三嗪基团类除草剂。在分析评估各合成工艺路线的基础上,研究了以2-羟基异丁酸甲酯先与氯化亚砜反应得到中间体氯代亚硫酰酯,在催化剂存在下再与氟化氢反应得到产品2-氟异丁酸甲酯的合成工艺,分析并实验优化了主要的合成工艺参数:氯化亚砜与2-羟基异丁酸甲酯的摩尔比为1∶1.7,氯化反应温度为-10~0℃,氯化反应时间为3~4h,收率达75%。
Methyl 2-fluoroisobutyrate, the key intermediates in the synthesis of triazine herbicides, was synthesized from methyl 2-hydroxyisobutyrate, thionyl chloride and fluorine hydride via esterification and fluorine substitution. The influences of esterification was investigated detailedly in molar ratio, temperature, reaction time and charging-up mode. Optimum reaction conditions were as follows: n(thionyl chloride):n(methyl 2-hydroxyisobutyrate) =1:1.7, -10-0℃, 3-4 h. The yield of Methyl 2-fluoroisobutyrate reached more than 75%.
出处
《农药》
CAS
北大核心
2008年第11期797-799,817,共4页
Agrochemicals