2-羟甲基-3,4-二甲氧基吡啶的高效合成  

Synthesis of 2-methyl-3-methoxy-4-chloropyridine with high yield

作　　者：夏家信 王从春 耿庆保 葛秀涛[2] 王永贵 李帅 邹智 任淑芝 杨志健 陈永旭 XIA Jiaxin;WANG Congchun;GENG Qingbao;GE Xiutao;WANG Yonggui;LI Shuai;ZOU Zhi;REN Shuzhi;YANG Zhijian;CHEN Yongxu

机构地区：[1]安徽金禾实业股份有限公司,安徽滁州239200 [2]滁州学院材料与化学工程学院,安徽滁州239000

出　　处：《淮南师范学院学报》2019年第2期146-148,共3页Journal of Huainan Normal University

基　　金：安徽省科技重大专项项目(16030801108);安徽省高校自然科学研究项目(KJ2017B05);国家级大学生创新创业训练项目(201810377018)

摘　　要：为解决PHC生产中由3,4-二甲氧基-2-甲基吡啶-N-氧化物与乙酸酐反应生成2-羟甲基-3,4-二甲氧基吡啶收率低、污染大、成本高的问题,采用一定量乙酸溶解3,4-二甲氧基-2-甲基吡啶-N-氧化物,使其以分子状态存在,并在一定温度和一定速度下滴加乙酸酐。结果表明,醋酸与3,4-二甲氧基-2-甲基吡啶-N-氧化物质量比1.0~1.2、乙酸酐滴加速率50.00~65.00 g/h、88℃下反应15 h,2-羟甲基-3,4-二甲氧基吡啶的收率是95.60%。根据液相色谱分析知含量94.94%,且验证了醋酸促进3,4-二甲氧基-2-甲基吡啶-N-氧化物与乙酸酐的反应。In order to solve the problem of low yield, high pollution and high cost of 2-methyl-3,4-dimethoxy pyridine produced by the reaction of 3,4-dimethoxy-2-methyl pyridine-N-oxide and acetic anhydride in PHC production, with a certain amount of acetic acid dissolved 3,4-dimethoxy-2-methyl pyridine-N-oxide exists in the molecular state, and acetic anhydride was added at a certain rate. The results show that the HAc and 3,4-dimethoxy-2-methylpyridine-N-oxide quality than 1.0 ~1.2, acetic anhydride drop speed rate is50-65 g/h, reaction after 15 h under 88℃. The yield of 2-hydroxy methyl-3,4-dimethoxy pyridine is 95.6%, the content of 94.94%,and promoted the 3,4-dimethoxy-2-methyl pyridine-N-oxide reaction with acetic anhydride.

关 键 词：PHC 醋酸 3 4-二甲氧基-2-甲基吡啶-N-氧化物 酰化 重排 

分 类 号：O69[理学—化学]