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直接使用CuCl2氯化芳基乙炔的反应通常存在着选择性差(有取代氯化和多种加成氯化的产物生成)、副产物多和分离困难等问题.描述了一种复合氯化剂(CuCl2·无机盐·载体)的制备以及基于该氯化剂取代氯化芳基乙炔的有效方法.首先通过一系列对比实验获得了CuCl2、载体和无机盐添加物的最佳配比.在此基础上考察了溶剂、复合氯化剂用量、反应温度诸因素对取代氯化反应的影响,提出了最佳反应条件:复合氯化剂为CuCl2·5/3Na Cl·5/2Al2O3,芳基乙炔与氯化剂的物质的量比为1∶3,溶剂为CH2Cl2,反应温度为35℃.在优化条件下,高产率(72%~99%)地合成了一系列1-氯-2-芳基乙炔目标产物1a~1n,并对这些化合物进行了表征.该方法反应条件温和、产率高、选择性好,并且适用于芳环上带有各种基团的底物.
Direct use of CuCl2 chloride aryl acetylene reaction usually exists the poor selectivity (with a variety of chlorinated and a variety of products of the formation of chlorinated), the problem of more by-products and separation difficult.Describes a complex chlorinating agent CuCl 2 · Inorganic salt · carrier) and an effective method based on this chlorination agent to replace aryl acetylene chloride.First, through a series of comparative experiments, the optimal ratio of CuCl 2, carrier and inorganic salt additive was obtained. The effects of various factors such as solvent, compounding chlorination agent and reaction temperature on the substitution of chlorination were investigated. The optimum reaction conditions were as follows: the complexing agent was CuCl2 · 5 / 3NaCl · 5 / 2Al2O3, The mass ratio of the chlorinating agent is 1: 3, the solvent is CH2Cl2 and the reaction temperature is 35 ° C. Under optimized conditions, a series of 1-chloro-2-aryl groups have been synthesized in high yields (72% ~ 99% Acetylene target products 1a ~ 1n were synthesized and characterized by these methods.The reaction conditions are mild, high yield, good selectivity and suitable for substrates with various groups on aromatic rings.