摘要
以间苯二酚为原料,经过成环、酯化、重排、开环4步反应,制得2,6-二羟基苯乙酮(1),对1进行了1HNMR表征,并对1的合成机理进行了推测;1与苯甲酰氯在相转移催化剂四丁基硫酸氢铵催化下进行反应,得到5-羟基黄酮(2),对2进行了IR及1HNMR表征,并对其合成机理进行了推测。考察了相转移催化反应温度、催化剂加入量对于产品收率的影响,较佳条件为:反应温度60℃,n(1)∶n(四丁基硫酸氢铵)=1∶1.3,2的收率达到65%。
Reaction of 2,6-dihydroxyacetophenone （1） with benzoyl chloride under phase-transfer catalysis by tetrabutyl ammonium bisulfate formed 5-hydroxyflavone （2） in 65% yield at 60℃ with n （1） ： n （tetrabutylammoniumbisulfate） = 1：1.3. 1 was synthesized from resorcinol in four steps including cyclization, esterification, rearrangement and ring-opening. The structures of 1 and 2 were identified by IR and 1H NMR. Mechanisms for formation of 1 and 2 were also proposed.
出处
《精细化工中间体》
CAS
2009年第5期47-49,共3页
Fine Chemical Intermediates
