3-氨基-4-氯苯甲酸十六酯的合成

systhnesis of hexadecyl 3-amino-4-chlorobenzoate

摘要:

以3-氨基-4-氯苯甲酸和正十六醇为原料，二甲苯为溶剂，对甲苯磺酸为催化剂酯化合成3-氨基-4-氯苯甲酸十六酯。采用傅里叶红外光谱（FTIR）、核磁共振光谱（NMR）的方法对产品的结构进行表征。考察了醇酸摩尔比、催化剂加量、反应物浓度对酯化率的影响。结果表明：醇酸摩尔比1.2:1，催化剂用量为总质量5%，反应物浓度65%，反应时间7 h，酯化率达96.20%，单程收率为73.91%。研究确立了产物提纯、提高单程收率和滤液去除催化剂后回收、重复使用的最佳系统工艺路线，单程收率提至78.90%，总收率为82.62%，产品的纯度高于使用标准。

Abstract:

Hexadecyl 3-amino-4-chlorobenzoate was synthesized by the esterification of 3-amino-4-chlorobenzoic and n-hexadecanol in the presence of p-toluenesulfonic acid as catalyst and xylene. as solvent. The products were characterized by FTIR, 1HNMR. The effects of molar ratio of acid to alcohol, the amount of catalyst, reacants' mass fraction on esterification rates were investigated. The optimal conditions were as followed: the molar ratio alkyd of achol to acid was 1.2:1,the catalyst was 5% of the total mass, the reacants' mass fraction was 65%, the esterification rate was 96.20%, and the one through yield was 73.91%. In addition, the best system route for product purification was estalished to improve one through yield and the filtrate recovery and reuse after removal of catalyst. The one through yield increased to 78.90%, the total yield was 82.62%, and the purity of the product was higher than 98.00%.