4-N,N-二甲氨基硫代苯甲酸合成工艺的研究

对以4-N,N-二甲氨基苯甲酰氯和NaHS为原料合成4-N,N-二甲氨基硫代苯甲酸 (DMATBA) 的工艺进行了研究，重点考察了反应溶剂种类、反应浓度、n (NaHS) : n (4-N,N-二甲氨基苯甲酰氯) 投料比、反应时间、反应温度、 n (NaHS) : n (HCl) 用量比，对产物收率的影响。实验结果表明，最佳的合成工艺为：反应溶剂DMF，反应浓度1.0 mol/L，n (NaHS) : n (4-N,N-二甲氨基苯甲酰氯) = 2:1，反应时间2.5 h，反应温度25 oC，n (NaHS) : n (HCl) = 1:1 (PH = 3)；经由酸化、萃取、减压蒸馏处理后，DMATBA总收率可达到82.1%，纯度为93.6%。

Study on the Synthetic Process of 4-N,N-dimethylaminothiobenzoic Acid

The process of synthesizing 4-N, N-dimethylaminothiobenzoic acid (DMATBA) with 4-N,N-dimethylaminobenzoyl chloride and NaHS as raw materials was studied, involving the influence of the type of reaction solvent, reaction concentration, n (NaHS): n (4-N,N-dimethylaminobenzoyl chloride) feed ratio, reaction time, reaction temperature and n (NaHS): n (HCl) dosage ratio on the yields of the product. The effects of solvent type, reaction concentration, n (NaHS) : n (4-N, N-Dimethylaminobenzyl Chloride) feeding ratio, reaction time, reaction temperature, n (NaHS) : n (HCl) dosage ratio of on product yield were investigated. Experimental results show that the best synthesis process in this screen involved reaction solvent DMF, reaction concentration 1.0 mol/L, n (NaHS): n (4-N,N-dimethylaminobenzoyl chloride) = 2:1, reaction time 2.5 h, reaction temperature 25 oC, n (NaHS): n (HCl) = 1:1 (PH = 3); after acidification, extraction, and vacuum distillation, the total yield of DMATBA can reach 82.1%, and the purity is 93.6%.