炔草酯的合成工艺研究  

Synthesis of Clodinafop-propargyl

作　　者：王述刚 蒋剑华 陈新春 薛谊 

机构地区：[1]南京红太阳生物化学有限责任公司,南京210047

出　　处：《现代农药》2016年第4期22-24,共3页MODERN AGROCHEMICALS

摘　　要：研究了以R-(+)-2-(4-羟基苯氧基)丙酸、氯丙炔、2,3-二氟-5-氯吡啶为原料,经由R-(+)-2-(4-羟基苯氧基)丙酸炔丙酯制备炔草酯的合成工艺,并讨论了溶剂、反应时间、反应温度对合成目标产物的影响。结果表明,以DMF为溶剂,碳酸钾为缚酸剂,在80℃左右条件下,R-(+)-2-(4-羟基苯氧基)丙酸与氯丙炔反应6 h,再升温到95℃左右,滴加2,3-二氟-5-氯吡啶反应10 h,过滤、重结晶得到炔草酯,收率达到89%,光学纯度为99%。Clodinafop-propargyl was synthesized via propargyl R-（＋）-2-（4-hydroxy phenoxy）propanoate by using R-（＋）-2-（ 4-hydroxyphenoxy） propionic acid, 3-chloro-propyne and 2, 3-difluoro-5-chloropyridine as starting materials. The influences of the solvent, reaction time temperature on the target product were investigated. Thus, R-（＋）-2-（4-hydroxy phenoxy）propionic acid reacted with 3-chloro-propyne for a period of 6 h at the temperature of 80℃ by using DMF as solvent and potassium carbonate as base to convert into the corresponding ester. Then, the resultant mixture was heated to about 95℃, 2,3-difluoro-5-chloropyridine was added dropwise and kept the reaction for 10 h, thus, via filtration and recrystallization, resulting in a yield of 89% for clodinafop-propargyl with 99% e.e.

关 键 词：炔草酯 合成 R-(+)-2-(4-羟基苯氧基)丙酸炔丙酯 除草剂 

分 类 号：TQ457.2[化学工程—农药化工]