以间二氯苯和甲醇钠为原料,对间氯苯甲醚合成的新工艺进行了研究; 通过单因素实验考察了溶剂种类及用量、间二氯苯与甲醇钠的摩尔比、反应温度、反应时间对间二氯苯转化率和间氯苯甲醚得率的影响,并采用正交实验法对反应条件进行了优化。确定了适宜的合成工艺条件为:以N,N-二甲基甲酰胺(DMF)作溶剂,溶剂用量为75 mL/mol,n(间二氯苯):n(甲醇钠)=1:1.2,反应温度为120 ℃,反应时间6 h。在此工艺条件下,间二氯苯的转化率为94.8%,间氯苯甲醚的得率为91.0%。采用FT-IR和GC-MS分析技术对间氯苯甲醚进行了表征。
Abstract
A new preparation process for m-chloroanisole was explored from 1,3-dichlorobenzene and sodium methoxide. The effects of types of solvent and their dosage, mole ratio of 1,3-dichlorobenzene to sodium methoxide, reaction temperature and reaction time on the conversion rate of 1,3-dichlorobenzene and yield of m-chloroanisole was examined. The optimum synthesis conditions were obtained by orthogonal test as follows: N, N-dimethyl-formamide(DMF)was used as solvent, and solvent dosage was 75 mL/mol; the molar ratio of 1,3-dichlorobenzene to sodium methoxide was 1:1.2; reaction temperature was 120 ℃ and reaction time was 6 h. Under this optimum conditions, the conversion rate of 1,3-dichlorobenzene was 94.8% and the yield of 1,3-chloroanisole was 91.0%. The structure of the m-chloroanisole was analyzed by FT-IR and GC-MS.
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基金
收稿日期:2014-09-15 修回日期:2015-04-24
基金项目:国家林业公益性行业科研专项项目(201104015); 国家自然科学基金项目(31170538)
第一作者:曹明珍,硕士生。*通信作者:王石发,教授。E-mail: wangshifa65@163.com。
引文格式:曹明珍,徐徐,鲍名凯,等. 间二氯苯合成间氯苯甲醚的工艺研究[J]. 南京林业大学学报:自然科学版,2015,39(5):150-154.
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