3-巯基-2-丁醇合成方法的改进及其异构体组成的分析鉴定  

Improved Synthesis of 2 Mercapto 3 butanol and Characterization of Its Isomers Component and Structure

作　　者：邢晓东[1] 唐国志[1] 方仁慈[1] 张树奎[1] 薜兵 

机构地区：[1]南开大学元素有机化学研究所

出　　处：《合成化学》1998年第4期408-412,共5页Chinese Journal of Synthetic Chemistry

摘　　要：以丁酮、氨、硫为原料，通过缩合反应合成２，４，５－三甲基－２－乙基噻唑啉－△３，再经水解、还原共三步反应合成了３－巯基－２－丁醇。考察了反应温度、催化剂、时间等因素对反应的影响，确定了优化条件：在３５℃进行缩合反应，以磷酸作为催化剂在３５℃下水解４ｈ，以ＫＢＨ４作为还原剂在２５℃下还原。简化了操作，缩短了反应时间，降低了成本，收率达５４％。通过ＧＣ，ＧＣ－ＭＳ。An improved method for the synthesis of 2 mercapto 3 butanol(Ⅴ) was reported.The influnce of temperature,time,catalysts,pH value on the yield of Ⅴ is studied.2 Butanone reacts with S powder and NH 3 gas in the molar proportions 2∶1∶1 at 35℃ for 7.5h to yield 2,4,5 trimethyl 2 ethylthiazoline △ 3(Ⅰ).Ⅰ is hydrolyzed to 3 mercapto 2 butanone(Ⅲ) by 10% H 3PO 4(aq.) at 35℃ for 4h.The title compoundd(Ⅴ) is obtained by hydrogenate Ⅲ with KBH 4 at 25℃.The total yield of Ⅴ reaches 54% on the base of 2 butanone.The component and structure of the end product are characterized by GC,GC MS and 1H NMR.

关 键 词：香料 巯基丁酮 三甲基 乙基噻唑 巯基丁醇 

分 类 号：TQ655[化学工程—精细化工] TS264.3[轻工技术与工程—发酵工程]