摘要
以对氨基水杨酸为起始原料,经过甲基化、硫氰化、还原乙基化、氧化、水解得到4-氨基-5-乙磺酰基-2-甲氧基苯甲酸。探讨了甲基化反应和硫乙基引入方法问题,并对各步反应合成条件进行了优化。改进后工艺总收率达55%,目标化合物和各中间体经IR,1 H NMR和MS等确证结构。
4-amino-5-(ethylsulfonyl) 2 methoxybenzoie acid is synthesized from amino salicylic acid via methylation, thiocyanation, reduction and ethylation, oxidation and hydrolysis reactions. The methylation reaction and the introduction method of ethyhhio group are investigated, and the reaction conditions of all steps are optimized. The total yield rate is 55 % after optimization, and the product and its intermediates are confirmed by IR, ^1H NMR and MS.
出处
《河北科技大学学报》
CAS
2014年第3期255-260,共6页
Journal of Hebei University of Science and Technology
基金
河北省自然科学基金(C2010000859)