3-二氯乙酰基-2，5-二甲基-2-正丙基-1，3-噁唑烷的合成工艺研究  

Synthesis of 3-Dichloroacetyl-2,5-dimethyl-2-n-propyl-1,3-oxazolidine

作　　者：付颖[1] 付宏刚[1] 叶非[2] 杨蕾[2] 李海涛[2] 

机构地区：[1]哈尔滨工业大学理学院应用化学系,黑龙江哈尔滨150001 [2]东北农业大学理学院应用化学系,黑龙江哈尔滨150030

出　　处：《高校化学工程学报》2008年第4期640-643,共4页Journal of Chemical Engineering of Chinese Universities

基　　金：黑龙江省自然科学基金项目(B200602);哈尔滨市科技创新人才研究专项资金项目(优秀学科带头人)(2007RFQXN017,2006RFXXN005);黑龙江省教育厅科学技术研究项目(11521038)

摘　　要：为了探索合成N-二氯乙酰基噁唑烷类除草剂安全剂的合成工艺,合成了3-二氯乙酰基-2,5-二甲基-2-正丙基-1,3-噁唑烷。以异丙醇胺、2-戊酮和二氯乙酰氯为原料,以氢氧化钠水溶液为缚酸剂,合成了标题化合物。采用红外光谱、核磁共振谱和元素分析对产品进行了结构表征。研究了合成过程中溶剂、反应温度、搅拌时间、摩尔比及缚酸剂对产物产率的影响,确定了合成标题化合物的较优反应条件为:以氢氧化钠为缚酸剂,三氯甲烷作溶剂,反应温度3～8℃,搅拌时间2h,异丙醇胺与2-戊酮的摩尔比为1:1.3,产率为50.0%。本方法原料价廉易得、路线简单、反应条件温和,适于工业化制备目标产物。In order to investigate the convenience synthetic route to synthesize N-dichloroacetyl oxazolidine compounds, a novel N-dichloroacetyl oxazolidine herbicide safener （3-dichloroacetyl-2,5-dimethyl-2-n-propyl- 1,3-oxazolidine） was synthesized. The title compound was synthesized from 1-amino-2-propanol, 2-pentanone and dichloroacetyl chloride, and NaOH aqueous solution of 33% was used as an acid attaching agent. The effects of solvent polarity, reaction temperature, stirring time and molar ratio of reactants on the yield of title compound were investigated. The optimum experimental conditions are as following： chloroform acts as solvent, reaction temperature is at 3-8℃, stirring time is 2 h and the molar ratio of 1-amino-2-propanol to 2-pentanone is 1：1.3. Using above reaction conditions, the yield is 50.0%. The structure of the title compound was characterized by IR spectrum, ^1H-NMR, ^13C-NMR and elemental analysis. The proposed synthetic route is simple, the reaction conditions are mild and the raw materials are cheap and easy to obtain.

关 键 词：除草剂安全剂 N-二氯乙酰基噁唑烷 合成 优化实验条件 

分 类 号：O626.24[理学—有机化学] TQ252.4[理学—化学]