逆酯型巯基酯的合成研究

Synthesis of Inverse Ester Mercaptoesters

介绍了一种以有机羧酸和巯基醇为原料合成逆酯型巯基酯的方法,以月桂酸和β-巯基乙醇为原料,对甲基苯磺酸作为催化剂,反应过程中利用抽负压的方法进行除水操作,以促进酯化反应进行完全,最终合成逆酯型月桂酸巯基乙酯为例进行研究。考察了各因素对酯化率的影响,得出最佳合成工艺条件:巯基乙醇投料系数为1.4,催化剂用量为巯基乙醇质量的4%。前期反应:温度80℃,真空度-0.045 MPa,反应3 h。后期反应:温度110℃,真空度为极限真空,反应4 h。在此工艺条件下反应合成的酯化率达97%以上。

This paper introduced a method for the synthesis of inverse ester of mercapto from organic carboxylic acid and mercaptoalcohol, in which lauric acid and beta-mercaptoethanol were used as raw materials and p-methyl benzene sulfonic acid was used as a catalyst, in the process of reaction, the method of vacuum extraction was used to remove water to promote the esterification reaction to complete, and finally the synthesis of reverse lauric acid mercaptoethyl ester was studied as an example. The effects of various factors on the esterification rate were investigated, and the optimum synthesis conditions were obtained as follows:(a) the feed coefficient of betamercaptoethanol was 1.4;the catalyst dosage was 4% of the mass of beta-mercaptoethanol;(b) the prophase of reaction:the temperature was 80 ℃, the vacuum was-0.045 MPa, the reaction time was 3 h.(c) The anap-phase reaction: the temperature was 110 ℃, the vacuum degree was the limit vacuum, the reaction time was 4 h. As a result, the esterification rate reached over 97% under the above conditions.