摘要
以水杨酸为原料合成5-溴-2-羟基3-(1-丙酰基)苯甲酸甲酯,从催化剂的用量、物料配比等方面研究了水杨酸甲酯化反应,以及从反应溶剂、加料方式和原料配比等方面研究了C-酰化反应,并利用IR、GC-MS确认产品结构。最佳工艺条件为:m(离子交换树脂催化剂):m(水杨酸)为1:100,n(甲醇):n(水杨酸)=7:1,氯仿为溶剂,加料方式为将酯滴加到氯化铝的氯仿溶液中,n(氯化铝):n(5-溴水杨酸甲酯):n(丙酸酐)=2:1:1,反应物总收率为74.52%。
5-Bromo-2-hydroxy-3-（1-propionyl） benzoic acid methyl ester was synthesized by using salicylic acid as raw material.The mass of catalyst,molar ratio of methanol to salicylic acid in the esterification,the effects of the solvent,feeding mode and molar ratio of reactants in the C-acylation were respectively investigated. The product was characterized by IR and GC-MS.The result indicated that the optimum technical conditions were as follows：m（ion exchange resin）：m（salicylic acid）=1.00%,n（methanol）：n（salicylic acid） = 7：1,chloroform as solvent;ester was added into the chloroform solution of aluminum chloride;n（aluminum chloride）：n（5- bromo-salicylic acid methyl ester）：n（propionic anhydride） = 2：1：1.Under these conditions,the total yield of desired product was 74.52%.
出处
《精细与专用化学品》
CAS
2010年第5期28-31,共4页
Fine and Specialty Chemicals
基金
国家科技支撑计划课题(2007BAI34B07)
国家自然科学基金(20776127)
浙江省自然科学基金(Y4090045)
浙江省自然科学基金杰出青年团队(R4090358)
浙江省教育厅科研项目(Y200908295)
