摘要
在蒸馏装置中无溶剂条件下，利用KF·2H2O作催化剂催化水杨醛类化合物与乙酰乙酸乙酯（或甲酯），通过Knoevenagel缩合反应快速简便地合成了5种3-乙酰基香豆素衍生物。探讨了催化剂用量和反应物摩尔比对合成3-乙酰基香豆素产率的影响，结果表明，水杨醛物质的量为20mmo]，水杨醛与乙酰乙酸乙酯（或甲酯）摩尔比为1：1．2，KF·2H2O用量为1．8mmol，反应30～35min，产率可达84．8％（或81．6％）；当用固态取代水杨醛代替水杨醛与乙酰乙酸乙酯（或甲酯）在摩尔比为1：2．0条件下反应时，得到4种3一乙酰基香豆素衍生物，产率达68．0％～87．3％（或63．5％～82．0％）。水杨醛苯环上有推电子基团时有利于提高反应产率。
KF · 2H2O was utilized as catalyst for synthesis of five kinds of 3 -acetyl coumarin derivatives by Knoevenagel condensation of salicylaldehyde and its derivatives with ethyl （or methyl ） aeetoacetate in distilling apparatus under solvent - free conditions. Effect of dosage of the catalyst and molar ratio of reactants on yield of 3 - acetyl coumarin was investigated. Results showed that yield of 3 - acetyl coumarin achieves 84. 8% （or 81.6% ） based on 20 mmol of salicylaldehyde, molar ratio of salicylaldehyde to ethyl （or methyl） acetoacetate 1： 1.2,dosage of KF · 2H2O 1.8 mmol and time of reaction 30 -35 min. When solid substituted salicylaldehyde displaces salieylaldehyde with ethyl （ or methyl） acetoacetate at a mole ratio of 1 ： 2.0, four kinds of 3 - acetyl coumarin derivatives were synthesized with the yield from 68.0% - 87.3% （or 63.5% - 82.0% ）. Substitution of electron donating groups on benzene ring of salicylaldehyde, such as diethyl amino - group, is favorable for improving yield of the condensation.
出处
《日用化学工业》
CAS
CSCD
北大核心
2013年第6期453-456,共4页
China Surfactant Detergent & Cosmetics
基金
梅州市科技局与嘉应学院资助项目(No.2012KJZ03)
作者简介
曾育才（1961-），男，广东梅州人，副教授，电话：13823838401，E-mail：mzzyc@jyu．edu．cn。
