炔草酯的合成工艺研究 |
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引用本文: | 王述刚,蒋剑华,陈新春,薛谊.炔草酯的合成工艺研究[J].现代农药,2016(4):22-24. |
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作者姓名: | 王述刚 蒋剑华 陈新春 薛谊 |
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作者单位: | 南京红太阳生物化学有限责任公司,南京,210047 |
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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%。
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关 键 词: | 炔草酯 合成 R-(+)-2-(4-羟基苯氧基)丙酸炔丙酯 除草剂 |
Synthesis of Clodinafop-propargyl |
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Abstract: | 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. |
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Keywords: | clodinafop-propargyl synthesis proparylR-(+)-2-(4-hydroxyphenoxy)propionate herbicide |
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