【摘要】 对以4-N,N-二甲氨基苯甲酰氯和Na HS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（Na HS） n（4-N,N-二甲氨基苯甲酰氯）投料比、反应时间、反应温度、n（Na HS） 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^-1,n（Na HS） 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℃，n（Na HS） n（HCl）=1 1（p H=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%.更多还原

【Abstract】 The process of synthesizing 4-N,N-dimethylaminothiobenzoic acid( DMATBA) with 4-N,Ndimethylaminobenzoyl 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 ℃,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%.更多还原