doi:10.16597/j.cnki.issn.1002-154x.2023.02.004
农药关键中间体2-氯-5-甲基吡啶的合成研究
丁永山∗ 陈洪龙 甘华军 王文魁 罗超然
(南京红太阳生物化学有限责任公司,江苏 南京 210047)
Study on the Synthesis of Pesticide Key Intermediate 2 - Chloro - 5 - methylpyridine
Ding Yongshan∗; Chen Honglong; Gan Huajun; Wang Wenkui; Luo Chaoran;
(Nanjing Red Sun Biochemical Co. , Ltd. , Jiangsu Nanjing 210047)
摘要:
以 2-氨基-5-甲基吡啶为原料,经过重氮化反应生成 2-氯-5-甲基吡啶。 考察了不同的亚硝酰氯制备方法、不同的反应温度、酸、溶剂对反应的影响。 实验结果表明:选择氯化亚砜、水、硝酸制备亚硝酰氯,15~20 ℃ 、 37% 的盐酸是 2-氨基-5-甲基吡啶最佳的重氮化反应条件,转化率 100%,收率可达 95%。
关键词：2-氨基-5-甲基吡啶；2-氯-5-甲基吡啶；2-羟基-5-甲基吡啶；重氮化反应；亚硝酰氯；
Abstract：
2 - chloro - 5 - methylpyridine was produced by diazotization from 2 - amino - 5 - methyl pyridine. The effects of different preparation methods of nitrosyl chloride, different reaction temperatures, acids and solvents on the reaction were investigated. The experimental results showed that the optimal reaction condition for diazotization of 2 - amino - 5 - methylpyridine was preparing nitrosyl chloride with sulfoxide chloride, water and nitric acid at 15 ~ 20 ℃ and using 37% hydrochloric acid. The conversion rate was 100% and the yield was 95% .
Keywords：2 - amino - 5 - methylpyridine; 2 - chloro - 5 - methylpyridine; 2 - hydroxy - 5 - methylpyridine; diazotization reaction; nitrite chloride;