摘要
为使富顺式二氯菊酸的合成方法更加方便、安全,以甲醇钠和叔丁醇为原料,用交换法合成叔丁醇钠,与3,3-二甲基-4,6,6,6-四氯己酸甲酯反应,得到富顺式二氯菊酸甲酯,进一步水解即可得富顺式二氯菊酸。最佳反应条件是:混合溶剂(叔丁醇:环己烷:二甲胺,38:35:15,v／v／v),碱用量(1.5:1,mol／mol),反应温度(-15℃--20℃),反应时间(3.5h)。反应所得二氯菊酸的顺反比可达6:4以上。
In order to make synthesis L1R-cis-permethrinic acid easier and safer, we prepared sodium tert-butoxide by an alcohol exchange reaction using tert-butyl alcohol and sodium methoxide, followed by reaction with methyl 3, 3-dimethyl-4, 6,6, 6-tetrachlorocaproate to produce cis-rich methyl permethrinate which was then hydrolyzed to perme-thrinic acid.Optimum reaction conditions were as follows: co-solvent of t-BuOH: cyclohexane : DMA (38 : 35 : 15 by vol), base ratio of 1.5 : 1, reaction temperature of - 15 to - 20℃ , and reaction time of 3.5 h. Under these conditions, the ratio of cis and trans isomers of methyl permethrinate exceeds 6 to 4.
出处
《农药》
CAS
北大核心
2004年第4期163-164,共2页
Agrochemicals
关键词
交换法
叔丁醇钠
富顺式
二氯菊酸
二氯菊酸甲酯
alcohol exchange reaction, sodium tert-butoxide, cis-rich, permethrinic acid, methyl permethrinate
