7-(二乙基氨基)-香豆素染料衍生物的合成工艺研究  

Synthesis Process of Derivative of 7-Diethylamino-coumarin Dye

作　　者：王跃东 王鲲鹏 WANG Yue-dong;WANG Kun-peng(College of Chemistry and Molecular Engineering,Qingdao University of Science and Technology,Qingdao 266045,Shandong China)

机构地区：[1]青岛科技大学化学与分子工程学院,青岛266045

出　　处：《染料与染色》2023年第3期11-14,共4页Dyestuffs and Coloration

摘　　要：为探究7-(二乙基氨基)香豆素二酮氟化硼衍生物的最佳合成工艺,采用单一变量实验法研究了溶剂、投料比、催化剂、反应时间及反应温度对产品收率的影响。结果表明:将原料4-(二乙基氨基)-水杨醛和4-羟基-6-甲基-2H-吡喃-2-酮按1∶1.2摩尔投料比、水作溶剂、L-脯氨酸作催化剂,80℃反应2 h得到中间体7-(二乙基氨基)香豆素的二酮产物,再将三氟化硼乙醚与中间体以3∶1摩尔投料、四氢呋喃作溶剂,25℃反应2 h得到最终产物。该工艺与以往文献方法相比有更高的收率,可达87%。Optimal synthesis conditions for diketone-difluoroboron derivative of 7-diethylamino-coumarin dye were investigated by sin-gle variable method.The effects of five variables including solvent,feed ratio,catalyst,reaction time,and reaction temperature on product yield were studied.The results showed that:the intermediate diketone derivative of 7-diethylamino-coumarin was obtained by using 4-diethylamino-salicylaldehyde and 4-hydroxy-6-methyl-2H-pyran-2-one as raw materials in a molar ratio of 1:1.2,water as the solvent,L-proline as the catalyst,and reacting at 80 C for 2 hours;the intermediate was reacted with boron trifluoride ether in a molar ratio of 1:3,using tetrahydrofuran as the solvent,and reacted at 25℃for 2 hours,and then,the final product was ob-tained.This method has a yield of up to 87%,which was higher than the yield reported in previous literatures.

关 键 词：香豆素 二酮氟化硼 染料 克莱森缩合反应 

分 类 号：TQ612.6[化学工程—精细化工]