豆田除草剂虎威的合成研究

Synthesis technique of soybean herbicide fomesafen

以间羟基苯甲酸和3,4-二氯三氟甲苯为起始原料,经过醚化、硝化和酰化三步反应合成虎威(氟黄胺草醚)。研究了虎威的合成工艺。试验表明,当温度为75℃~80℃、反应时间为3.5 h^4.5 h、摩尔比为n(三氟羧草醚)∶n(甲基磺酰胺)∶n(三氯氧磷)=1∶1.03∶1.62时,产品收率可达91.7%。对合成的氟磺胺草醚经过精制处理,其纯度为98.5%。该生产工艺可以降低成本,适于工业化生产。

Fomesafen, was synthesized via condensation, nitration and acylation using m-hydroxybenzoic, 3, 4-dichlorlde-trifluoridemethylbenzene as starting reagents. The synthesis technology of fomesafen was researched. The experiment showed that at 75 ℃～ 80 ℃, a reaction time of 3.5 h-4.5 h, a molar ratio for n （acifluorfen） ： n （methylsulfoamide） ： n （trichloridephosphorusoxid） = 1 ： 1.03：1.62, the product yield was 91.7 %. When the synthesized fomesafen was first put through a purification treatment, the purity was 98.5 %. Both quality and yield were consistent across batches. Thus, this process provided a lower energy consumption production technology and was suitable for industrial scale manufacturing.