1-(4-氯苯基)-4,4-二甲基-1-烯-3-戊酮的合成工艺优化  

Synthesis Optimization of 1-(4-Chlorophenyl)-4,4-dimethylpent-1-ene-3-one

作　　者：吴伟 方燕[1] 叶振君 韩海平 徐海燕 张芝平 毕强 李忠 WU Wei;FANG Yan;YE Zhenjun;HAN Haiping;XU Haiyan;ZHANG Zhiping;BI Qiang;LI Zhong(Shanghai Shengnong Pesticide Co., Ltd., Shanghai 201619, China;East China University of Science and Technology, Shanghai 200137, China)

机构地区：[1]上海生农生化制品股份有限公司,上海201619 [2]华东理工大学,上海200137

出　　处：《世界农药》2019年第1期49-51,57,共4页World Pesticide

基　　金：上海市优秀技术带头人计划资助项目(16XD1422300);上海市人才发展资金资助项目(2017108)

摘　　要：通过对氯苯甲醛和频哪酮羟醛缩合反应的条件优化,减少歧化杂质,提高原料转化率。以对氯苯甲醛和频呐酮为原料,在强碱性催化作用下反应得到烯酮产品[化学名:1-(4-氯苯基)-4,4-二甲基-1-烯-3-戊酮]。通过反应条件优化,试验确定的最佳反应条件是:反应温度为45℃,对氯苯甲醛1.0 eq,频哪酮1.10 eq,以甲醇为反应溶剂。母液套用5次,平均收率为96.4%,产品含量为98%。烯酮合成工艺优化后得到的条件收率高,歧化杂质明显减少,有较好的工业应用价值。This paper aimed to improve the conversion of raw materials and reduce disproportionation impurities by optimizing reaction condition. With p-chlorobenzaldehyde and pinacolone as raw materials and methanol as solvent, they reacted under strong basic catalysis to give ketene. With the optimal reaction conditions, the product was synthesized with 1.10 eq pinacolone under 45oC, and methanol was recycled for five times. The average yield of product reached 96.4% with the purity of 98%. The disproportionation impurities were obviously reduced.

关 键 词：烯酮 对氯苯甲醛 频呐酮 

分 类 号：TQ450[化学工程—农药化工]