3,5,6-三氯吡啶-2-醇钠的合成

Synthesis of Sodium 3,5,6-Trichloropyridin-2-ol

[目的]对传统"一锅法"合成三氯吡啶醇钠的工艺进行探索和优化。[方法]以三氯乙酰氯和丙烯腈为原料,在混合溶剂和复合催化剂存在下,于一个反应釜中经加成环合及芳构化反应,过滤,精制得到3,5,6-三氯吡啶-2-醇钠成品。[结果]最佳工艺条件:助催化剂的复配比为1∶0.20~0.35,三氯乙酰氯与丙烯腈物质的量之比为1∶1.4~1.6,反应温度为110~130℃,反应时间为10~14 h。[结论]优化工艺条件后,三氯吡啶醇钠的合成收率达到82.0%以上,含量达到88.0%,且反应时间较传统工艺减少50%。

[Aims] The study aims to research and optimize the conventional process of the sodium 3,5,6-trichloropyridin-2-ol via one-pot. [Methods] The product sodium 3,5,6-trichloropyridin-2-ol was synthesized via one-pot in the presence of mixed solvent and composite catalyst, using trichloroacetyl chloride and acrylonitrile as the raw materials through reactions of addtiion, cyclization, aromatization, filtration and purification. [Results] The optimal process condition was that the composited ratio of co-catalyst was 1 ∶0.20-0.35, the mole ratio of trichloroacetyl chloride to acrylonitrile was 1∶1.4-1.6, the reaction temperature and time were 110-130 ℃ and 10-14 h, respectively.[Conclusions] It was concluded that the total yield of the product sodium 3,5,6-trichloropyridin-2-ol was more than82.0% and the purity was 88.0%, at the same time, reaction time were saved by 50% with the novel optimized process.