摘要
为解决PHC生产过程中由2-甲基-3-甲氧基吡啶酮与三氯氧磷反应生成2-甲基-3-甲氧基-4-氯吡啶的收率低、污染大、成本高的问题,本研究以偶极矩大的1,2-二氯乙烷(D=6.20)替代偶极矩小的二氯甲烷(D=3.80)作溶剂,并将三氯氧磷改为一定速度的滴加。实验结果表明:1,2-二氯乙烷与2-甲基-3-甲氧基吡啶酮的最佳质量比为7.5、三氯氧磷的滴加速率为40g/h,在85℃下反应10h,通过减压旋蒸和萃取,得到的产物2-甲基-3-甲氧基-4-氯吡啶的收率为98.02%,含量97.59%。说明大极性溶剂1,2-二氯乙烷更有利于烯醇式结构体(2-甲基-3-甲氧基-4-羟基吡啶)的存在和含量的提升,从而促进了2-甲基-3-甲氧基-4-氯吡啶的生成。
To solve the problems of low yield,serious pollution and high cost of PHC production by the reaction of and phosphorus oxychloride.We replaced the dichloromethane with1,2-dichloroethane as solvent,and changed the addition way of abundant phosphorus oxychloride with droping under a certain rate.The results demonstrated that the optimal mass ratio between 1,2-dichloroethane and 2-methyl-3-methoxy Pyridone was 7.5.The droping rate of phosphorus oxychloride was 40 g/h,and the reaction spent 10h under 85℃.Moreover,the product of 2-methyl-3-methoxy-4-chlorine pyridine was obtained by reduced pressure distillation and extraction with yield of 98.02%and content of 97.59%.In contrast with dichloromethane with larger polarity,the low polar 1,2-dichloroethane is more beneficial to existence of enol structure(2-methyl-3-methoxy-4-hydroxy pyridine)and improvement of content,and synthesis of 2-methyl-3-methoxy-4-chlorine pyridine with phosphorus oxychloride.
作者
夏家信
王从春
耿庆保
葛秀涛
王永贵
王晓宇
訾锦达
任淑芝
杨志健
陈永旭
Xia Jiaxin;Wang Congchun;Geng Qingbao;Ge Xiutao;Wang Yonggui;Wang xiaoyu;Zijinda;Ren Shuzhi;Yang Zhijian;Chen Yongxu
出处
《滁州学院学报》
2018年第5期54-56,共3页
Journal of Chuzhou 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)
滁州学院大学生创新创业训练项目(2018CXXL048)
