苯达松合成工艺的研究  

Study on the synthesis of bentazone

作　　者：杨旭 卢福军 周长海 唐晓婵[1,2] 邢伶 岳涛 YANG Xu;LU Fu-jun;ZHOU Chang-hai;TANG Xiao-chan;XING Ling;YUE Tao(Shandong Chemical Technology Academy of Qingdao University of Science&Technology,Jinan 250014,China;Organic Reaction in Aqueous Engineering Research Center of Shandong Province,Jinan 250014,China)

机构地区：[1]青岛科技大学山东化工研究院,山东济南250014 [2]山东省水相有机合成及高效清洁分离工程技术研究中心,山东济南250014

出　　处：《应用化工》2022年第S01期77-81,共5页Applied Chemical Industry

基　　金：山东省“泰山学者”建设工程基金(08190201)项目。

摘　　要：以邻氨基苯甲酰异丙胺为起始原料,三氧化硫为磺化剂,在二氯乙烷溶剂下制备邻氨基磺酸苯甲酰异丙胺中间体,在三氯氧磷催化下中间体闭环反应生成苯达松。苯达松反应液经碱溶酸化、干燥等后处理得到苯达松固体。考察了物料摩尔比、反应温度、反应时间、三氧化硫络合剂等因素对中间体合成的影响,结果表明,三氧化硫摩尔比为1.2,反应温度为80℃,反应时间为30 min,邻氨基苯甲酰异丙胺转化率>99%,中间体选择性>99%。中间体合成苯达松过程,考察了催化剂、物料摩尔比、反应温度、反应时间、三氧化硫络合剂对苯达松合成的影响,以三氯氧磷为催化剂,三氯氧磷摩尔比为1.1,反应为85℃,反应时间为2 h,三氧化硫络合剂为2-甲基吡啶,邻氨基苯甲酰异丙胺转化率为99%,整个工艺苯达松收率为85%。Using o-aminobenzoyl isopropylamine as starting material,sulfur trioxide as sulfonating agent,the intermediate of o-aminosulfonic acid benzoyl isopropylamine was prepared in dichloroethane solvent.The closed-loop reaction of the intermediate was catalyzed by phosphorus oxychloride to form bentazone.Bentazone solid was obtained from bentazone reaction solution after alkali solution acidification and drying.The effects of molar ratio of materials,reaction temperature,reaction time and sulfur trioxide complexing agent on the synthesis of intermediates were investigated.The results showed that when the molar ratio of sulfur trioxide was 1.2,reaction temperature was 80℃,reaction time was 30 min,the conversion of o-aminobenzoyl isopropylamine was more than 99%,and the selectivity of intermediates was more than 99%.The effects of catalyst,molar ratio of materials,reaction temperature,reaction time and sulfur trioxide complexing agent on the synthesis of bendazone were investigated.Phosphorus oxychloride was used as catalyst,the molar ratio of phosphorus oxychloride was 1.1,the reaction temperature was 85℃,the reaction time was 2 h,the sulfur trioxide complexing agent was 2-methylpyridine,and the conversion of o-aminobenzoyl isopropylamine was 99%,the yield of bendazone was 85%.

关 键 词：邻氨基苯甲酰异丙胺 邻氨基磺酸苯甲酰异丙胺 三氧化硫络合剂 三氯氧磷 

分 类 号：TQ203[化学工程—有机化工]