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 usin...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.展开更多
在二氯乙烷溶剂中采用N,N-二甲基甲酰胺作催化剂,苯磺酸钠与双(三氯甲基)碳酸酯(BTC)反应制备苯磺酰氯,然后肼解得到苯磺酰肼.研究了催化剂、溶剂和BTC用量对苯磺酰氯收率的影响,优化条件下氯化反应收率为90.8%;此外,对肼解反应滴加温...在二氯乙烷溶剂中采用N,N-二甲基甲酰胺作催化剂,苯磺酸钠与双(三氯甲基)碳酸酯(BTC)反应制备苯磺酰氯,然后肼解得到苯磺酰肼.研究了催化剂、溶剂和BTC用量对苯磺酰氯收率的影响,优化条件下氯化反应收率为90.8%;此外,对肼解反应滴加温度和反应温度对苯磺酰肼收率的影响进行了考察.优化条件下,苯磺酰肼两步总收率81.9%,其结构经1 H NMR和IR表征确认.采用BTC代替三氯氧磷作氯化试剂,操作安全,并可避免含磷废水对环境的影响,是一种绿色环保的工艺.展开更多
文摘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.
文摘在二氯乙烷溶剂中采用N,N-二甲基甲酰胺作催化剂,苯磺酸钠与双(三氯甲基)碳酸酯(BTC)反应制备苯磺酰氯,然后肼解得到苯磺酰肼.研究了催化剂、溶剂和BTC用量对苯磺酰氯收率的影响,优化条件下氯化反应收率为90.8%;此外,对肼解反应滴加温度和反应温度对苯磺酰肼收率的影响进行了考察.优化条件下,苯磺酰肼两步总收率81.9%,其结构经1 H NMR和IR表征确认.采用BTC代替三氯氧磷作氯化试剂,操作安全,并可避免含磷废水对环境的影响,是一种绿色环保的工艺.
