摘要
以对氨基水杨酸为起始原料,用硫酸二甲酯甲基化制得4-氨基-2-甲氧基苯甲酸甲酯;然后与溴素和硫氰酸钾反应制得4-氨基-2-甲氧基-5-氰硫基苯甲酸甲酯;再用溴乙烷在氢氧化钾催化下乙基化制得4-氨基-5-乙硫基-2-甲氧基苯甲酸;最后用双氧水氧化制得氨磺必利的中间体4-氨基-5-乙磺酰基-2-甲氧基苯甲酸,合成总收率为24.5%,目标物化学结构经IR、1HNMR、MS确证。
The 4-amino-5-ethylsulfonyl-2-methoxybenzoic acid, an intermediate of amisulpride was synthesized from 4-amino-2-hydroxybenzoic acid as material, Firstly, the methyl 4-amino-2-methoxybenzoate was obtained by the methylation of dimethyl sulfate, Then, the methyl 4-amino-2-methoxy-5- thiocyanatobenzoate was prepared by the reaction of potassium thiocyanate with bromine. Furthermore, the methyl 4-amino-5-ethyhhio-2-methoxy benzoicaeid was formed from the ethylation of bromoethane at catalysis of potassium hydroxide. Finally, the 4-amino-5- ethylsulfonyl-2-methoxybenzoic acid was obtained via oxidation with hydrogen peroxide. The total yield was 24.5%. The chemical structure was confirmed by IR, ^1H NMR, MS.
出处
《精细化工中间体》
CAS
2008年第3期29-32,共4页
Fine Chemical Intermediates
