【作者】 章凯丽； 杜晓华；

【Author】 ZHANG Kai-li;Du Xiao-hua;Catalytic Hydrogenation Research Center, Zhejiang Key Laboratory of Green Pesticides and Cleaner Production Technology, Zhejiang University of Technology;

【机构】 浙江工业大学催化加氢研究中心浙江省绿色农药清洁生产技术研究重点实验室；

【摘要】 [目的]利用乙氧氟草醚副产物2-氯-4-三氟甲基苯酚制备乳氟禾草灵。[方法]用2-氯-4-三氟甲基苯酚与双（三氯甲基）碳酸酯（BTC）制备中间体双（2-氯-4-三氟甲基苯基）碳酸酯,然后在缚酸剂存在下,与O-[5-氯-2-硝基苯甲酰基]乳酸乙酯进行缩合反应得到乳氟禾草灵,并对各反应条件进行优化。[结果]滴加温度和保温温度均为100℃,碳酸钾为碱,n（K₂CO₃）:n（O-[5-氯-2-硝基苯甲酰基]乳酸乙酯）:n（双（2-氯-4-三氟甲基苯基）碳酸酯）的投料比为2.15:1:0.56,DMF（除水）为最佳溶剂,反应时间10 h,收率和纯度分别为81.3%和98.1%。[结论]利用乙氧氟草醚副产物制备乳氟禾草灵,降低生产成本,减少环境污染,具有工业化应用前景。更多还原

【Abstract】 [Aims]A new method for preparation of lactofen using oxyfluorfen’s by-product of2-chloro-4-trifluoromethylphenol.[Methods]Intermediate of bis（2-chloro-4-trifluoromethylphenyl）carbonate was prepared by reacting 2-chloro-4-trifluoromethylphenol with bis（trichloromethyl）carbonate（BTC）,and then reacted with ethyl 0-[5-fluoro-2-nitrobenzoyl]lactate to obtain lactofen in the deacid reagent of potassium carbonate.The synthesis conditions were optimized.[Results]Dropping temperature and holding temperature were 100℃,potassium carbonate as a base,raw material feed ratio of n（K₂ CO₃）:n（ethyl 0-[5-chloro-2-nitrobenzoyl]lactate）:n（bis（2-chloro-4-trifluoromethylphenyl）carbonate）was 2.15:1:0.56,DMF（water removal）was the best solvent,react time was 10 h.The yield and purity were obtained in 81.3% and 98.1%.[Conclusions]A synthetic method of lactofen using oxyfluorfen’s by-product has such advantages of reduce production cost and environmental pollution.The method is suitable for industrial production.更多还原