氟草烟异辛酯的合成研究

Synthesis of Fluroxypr-mepthyl

标题化合物是一种含氟高效、低毒、低残留的吡啶类除草剂,广泛应用于防除阔叶类杂草。以2,3,4,5,6-五氯吡啶为原料,通过氟代、氨化、水解,再与氯乙酸甲酯缩合,最后在氯酞酸四丁酯催化下与仲辛醇发生酯交换反应来制备标题化合物。4步反应总收率77.3%,产物纯度99.5%,化合物结构经过1HNMR和13CNMR确证。其中所用的溶剂和催化剂均可回收套用,减少了对环境的污染。此外,氨化和水解反应一锅法完成。工艺条件温和、操作简单、成本低,适合工业化生产。

The title compound is a fluorine-containing pyridine herbicide with high efficiency,low toxicity and low residue,which is widely used in broad-leaved weeds.2,3,4,5,6-Pentachloropyridine was used as raw materials to prepare the title compound by fluorination,amination,hydrolysis and condensation with methyl chloroacetate followed by transesterification with sec-octanol under the catalysis of tetrabutyl chlorotitanate.The total yield of the 4-step reaction with a purity of 99.5%,and an overall yield of 77.3%,and the structure of the compound was confirmed by 1HNMR and 13CNMR.The solvent and catalyst used can be recycled,and used to reduce environmental pollution.Besides,amination and hydrolysis were completed in one pot.The process condition was mild,simple in operation,and was suitable for industrialized production.