碳酸二甲酯甲基化合成乙酰甲氧胺的反应研究  

Study on synthesis of acetyl methamphetamine with as methyl carbonate as methyl reagents

作　　者：申宏丹[1] 朱驯[1] 项东升[1] 王群 王涛 SHEN Hongdan;ZHU Xun;XIANG Dongsheng;WANG Qun;WANG Tao(Yancheng Industry Vocational Technology College,Yancheng 224005,China;Yancheng Lüzhou Technology Co.Ltd.,Yancheng 224005,China)

机构地区：[1]盐城工业职业技术学院,江苏盐城224005 [2]盐城市绿洲环保科技有限公司,江苏盐城224005

出　　处：《印染助剂》2022年第2期23-26,共4页Textile Auxiliaries

基　　金：江苏省产学研合作项目;江苏省大学生实践创新项目(202013752029Y)。

摘　　要：用绿色化学原料碳酸二甲酯(DMC)代替硫酸二甲酯(DMS)等传统有毒有害试剂作为甲基化试剂、以1,8-二氮杂二环十一碳-7-烯(DBU)作为催化剂、聚乙二醇(PEG-600)作为相转移催化剂,研究DMC与乙酰羟胺的甲基化反应。考察物料配比、反应时间、反应温度等因素对反应的影响,得到的优化反应条件为:n(乙酰羟胺)∶n(DMC)∶n(PEG-600)∶n(DBU)=1.00∶2.00∶0.12∶0.80,反应温度120℃,反应时间6 h,收率最高可达78.1%,转化率为99.3%。Use the green chemical raw material dimethyl carbonate(DMC) instead of traditional toxic and harmful reagents dimethyl sulfate(DMS) as methylation reagents. With 1,8-diazabicyclo[5.4.0] undec-7-ene(DBU) as the catalyst, polyethyl glycol(PEG-600) as the phase transfer catalyst, the methylation reaction of DMC and acetylamide was studied. The effects of material ratio, reaction time, reaction temperature, etc. on the reaction were investigated. The optimized reaction conditions were as follows: n(acetylamide)∶n(DMC)∶n(PEG-600)∶n(DBU)=1.00∶2.00∶0.12∶0.80, reaction temperature 120 ℃, reaction time 6 h. The highest yield was 78.1%, and the conversion rate was 99.3%.

关 键 词：碳酸二甲酯 DBU催化 绿色合成 乙酰甲氧胺 

分 类 号：TQ225.5[化学工程—有机化工]