3,5,6-三氯吡啶-2-酚的合成优化

Optimization on Synthesis Technology of 3,5,6-Trichloropyridine-2-phenol

[目的]进一步优化三氯乙酰氯合成三氯吡啶酚的工艺。[方法]以三氯乙酰氯、丙烯腈为原料,在催化剂作用下,通过加成环化、芳构化2步法合成3,5,6-三氯吡啶-2-酚,考察溶剂类型、催化剂用量、助催化剂类型和反应压力对三氯吡啶酚收率的影响。[结果]三氯乙酰氯路线合成三氯吡啶酚的优化工艺为:三氯乙酰氯、丙烯腈为原料,1.3 g/46 g(三氯乙酰氯)氯化亚铜为催化剂,二氯苯为溶剂,此条件下三氯吡啶酚的收率可达55%。微负压条件有利于及时排除反应过程中产生的氯化氢,降低安全隐患,而添加助催化剂对反应效果无显著促进作用。[结论]该研究确定了三氯乙酰氯路线合成三氯吡啶酚的最佳工艺。

[ Objective ] The purpose was to further optimizing the synthesis technology of trichloropyridine phenol from trichloro-acetie chloride. [ Method] With trichloro-aeetie chloride and acrylonitrile as raw materials,under the action of catalyst,3,5,6- trichloropyridine-2-phenol was synthesized through 2 steps of adding cyclization and aromatization and the influences of solvent types,catalyst dosage,promoter types and response pressure on the yield rate of trichloropyridine phenol were investigated. [ Result] The optimized synthesis technology of trichioropyridine phenol from trichloro-acetic chloride was that under the condition with trichloro-acetic chloride and acrylonitrile as raw materials, 1.3 g/46 g （trichloro-acetic chloride） cuprous chloride as catalyst and diehloro-benzene as solvent, the yield rate of triehloropyridine phenol could reach 55%. Micro negative pressure was favorable to deplete chloride hydrogen produced from reaction timely so as to decrease hidden danger. And the addition of promoter had no promotiug action on reaction effect. [ Conclusion I The optimum synthesis technology of trichloropyridine phenol from trichloro-acetie chloride was confirmed in this research.