3,5,6-三氯吡啶-2-酚的合成与波谱特征

来源期刊：中南大学学报(自然科学版)2000年第1期

论文作者：曹育才 蒋玉仁 薛玉兰 曹学锋 周立辉

文章页码：24 - 26

关键词：3,5,6-三氯吡啶-2-酚;合成;红外光谱;质谱

Key words：3,5,6-trichloropyridin-2-ol; synthesis; IR spectrum; MS spectrum

摘    要：以CuCl/Cu作催化剂,采用三氯乙酰氯与丙烯腈加成,在常压条件下合成了较高收率的3,5,6-三氯吡啶-2-酚.研究了催化剂种类对合成收率的影响,并通过实验确定了合成工艺条件:M(CuCl/Cu)=4·5 g·mol^-1,M(NB)=134 g·mol^-1,摩尔比n(AN)/n(TCAO)=1·2,反应时间17 h,反应温度160℃.3,5,6-三氯吡啶-2-酚的红外光谱和质谱完全表明了其结构特征.

Abstract: 3,5,6-trichloropyridin-2-ol(TCPO) can be synthesized conveniently through CuCl/Cu catalyzed addition between trichloroacyl chloride (TCAC) and acrylonitrile(AN). The effects of different catalysts on the recovery of TCPO were investigated, and the optimized synthetic process of TCPO was obtained experimentally as follows: CuCl/Cu present as a catalyst with the dosage of 4.5 g·mol^-1; solvent nitribenzene 134 g·mol^-1;n(AN)/n(TCAC)=1.2 (molar ratio); reaction time is 17 h and reaction temperature is 160℃. Furthermore, the molecular structural characteristics of TCPO were discussed through IR and MS spectrum.