超高效除草剂氟噻乙草酯的清洁生产工艺

A clean process with 3 steps for the synthesis of Fluthiacet-methyl as a super effective herbicide is developed.The product was prepared in several patented methods.However, those methods had the disadvantages of using hazardous materials such as thiophosgene, chloroformate, hexahydropyridazine and phosgene.In the present work, the hazardous materials were replaced by safe reagents,for example, thiophosgene by carbon disulfide, chloroformate and phosgene by bis(trichloromethyl) carbonate(BTC) and hexahydropyridazine by hexahydropridazine hydrochloride.Therefore, the process is operationally convenient and safe with little environmental hazard.Furthermore, the total yield (63%) is quite higher than that (39%) reported in literature.The clean process is valuable for manufacturing Fluthiacet methyl in industrial scale.

浙江新农化工股份有限公司氟噻乙草酯通过省级验收

受浙江省经济贸易委员会委托。

超高效液相色谱-串联质谱法测定玉米、大豆和土壤中的氟噻乙草酯残留

建立玉米、大豆和土壤中氟噻乙草酯残留的液质串联快速分析检测方法。样品中的氟噻乙草酯经乙腈提取,N-丙基乙二胺（PSA）和多壁碳纳米管（MWCNTs）净化,利用超高压液相色谱-串联质谱（UPLC-MS/MS）在多反应监测模式下进行检测。以碎片离子对404.0/274.0定性、离子对404.0/344.0进行外标法定量。仪器在0.001-1.0 mg/kg范围内,具有良好线性关系。在0.001-1.0 mg/kg添加水平范围内,氟噻乙草酯在玉米、大豆和土壤中的平均回收率为95.8%-105.0%,变异系数为3.1%-7.8%。该方法的检出限（LOD）为0.007-0.014μg/kg,定量限为（LOQ）为1.0μg/kg。本方法简便、快速、准确,能满足国内外法规的要求,可用于玉米、大豆和土壤样品中氟噻乙草酯的农药残留确证检测。

超高效除草剂氟噻乙草酯

氟噻乙草酯是由日本组合化学公司研制,并与诺华公司(现为先正达公司)共同开发的酰亚胺类除草剂。以邻氟苯胺为起始原料,经酰化、氯化制得中间体4-氯-2-氟乙酰苯胺,再与氯磺酸反应后经还原、水解制得中间体取代的硫酚,经醚化,制成硫代异氰酸酯,最后与肼缩合,并与光气合环即得目的物。主要用于玉米田、大豆田防除阔叶杂草,使用剂量为5～10g a.i./hm2。

8-硫-1,6-二氮双环[4.3.0]壬烷-7,9-二酮的合成及单晶结构

以二硫化碳、甲醇、氢氧化钾为起始原料,经3步反应生成5-甲氧基-1,3,4-噻二唑-2(3H)-酮,再与1,4-二溴丁烷进行取代,然后脱甲基,最后发生亲核取代反应得到8-硫-1,6-二氮双环[4.3.0]壬烷-7,9-二酮。通过熔点、1HNMR、13CNMR、元素分析及X射线衍射分析等方法对产物的结构进行了表征,目标化合物属于三斜晶系,P1空间群,晶胞参数a=0.784 00(16)nm,b=1.046 4(2)nm,c=1.051 4(2)nm,α=63.84(3)°,β=79.62(3)°,γ=89.42(3)°,V=0.759 2(3)nm3,Z=4,wR(F2)=0.125,μ=0.37 mm-1。