3,5,6-三氯-2-吡啶酚的合成工艺研究

Studies on Synthesis of 3,5,6-Trichloropyridin-2-ol

在混合溶剂、复合催化剂及原料配比上对 3,5 ,6 三氯 2 吡啶酚的合成工艺进行改进 ,同时通过单因素实验和正交实验优化反应工艺 ,当氯化亚铜和B以质量比 1∶0 1 5组成复合催化剂 ,硝基苯和溶剂A以体积比 3 5∶1组成混合溶剂 ,三氯乙酰氯与丙烯氰摩尔比为 1 4,反应时间 1 2h ,氢氧化钠质量分数为 30 % ,3,5 ,6 三氯 2 吡啶酚 (TCPO)的收率达 71 0 %。通过红外光谱和色质联用仪分析确定了其结构 ,测定其纯度为 97 9%。

3,5,6-Trichloropyridin-2-ol(TCPO)was synthesized using trichloroactyl chloride and acrylonitrile as raw materials,nitrobenzene and A as solvent and B and CuCl as catalyst.When n(trichloroactyl chloride)∶n(acrylonitrile)was 1.4∶1,V(nitrobenzene)∶V(compound A)was 3.5∶1, m(CuCl)∶m(B)was 1∶0.15 and reaction time was 12 h, the yield and purity of product were 71% and 97.9% respectively. The structures of products and main impurities were confirmed by FT-IR and GC-MS.