对甲氧基苯甲酸的合成工艺研究

Study on Synthetic Process of p-Methoxybenzoic Acid

以对羟基苯甲酸为起始原料,采用一锅法合成工艺,考察了氢氧化钠、硫酸二甲酯、反应温度和反应时间对反应产率的影响.最佳反应条件为:反应温度为40℃,滴加1 h后继续反应1 h,对羟基苯甲酸、硫酸二甲酯和NaOH的物质的量比为1∶1.5∶3.0,收率达94.0%.其结构通过1H NMR确证.

The synthetic process of p-methoxybenzoic acid was studied by one pot process method of 4-hydroxybenzoic acid and dimethyl sulfate.The effects of various technical parameters,such as NaOH and dimethylmonosulfate agent dosage,reaction temperature and time were investigated by single factor method.And finally a product yield of 94.0% could be achieved under the conditions as follows:the equivalent molar ratio of 4-hydroxybenzoic acid to NaOH and dimethylmonosulfate was 1∶3.0∶1.5,reaction temperature,drip time and reaction time were 40 ℃,1 h and 1 h,respectively.Its structure was characterized by 1H NMR.