炔草酯的合成工艺研究

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%。

Synthesis of Clodinafop-propargyl

Clodinafop-propargyl was synthesized via propargylR-(+)-2-(4-hydroxy phenoxy)propanoate by usingR-(+)-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.