磷钨酸催化合成1,3-二硫杂环戊烷类香料化合物  

Synthesis of Flavoring Compounds 1, 3- Dithiolanes Catalyzed by Phosphotungstic Acid

作　　者：郑福平[1] 李海军[1] 孙宝国[1] 谢建春[1] 刘玉平[1] 田红玉[1] 

机构地区：[1]北京工商大学化学与环境工程学院,北京100037

出　　处：《中国食品学报》2006年第1期63-66,共4页Journal of Chinese Institute Of Food Science and Technology

基　　金：国家自然科学基金资助项目(No.20376003)

摘　　要：以磷钨酸为催化剂,乙二硫醇与异戊醛在苯中回流,合成了2-异丁基-1,3-二硫杂环戊烷。研究了乙二硫醇与异戊醛物质的量比、催化剂用量、反应时间等因素对反应收率的影响。优化条件为:乙二硫醇与异戊醛投料物质的量比为1.8,催化剂用量占反应物料总质量的2.0%,反应时间2.5h。按类似条件合成了2-甲基-2-丁基-1,3-二硫杂环戊烷、1,4-二硫杂螺[4.4]壬烷、(2′-甲基-1′,3′-二硫杂-2-环戊基)乙酸乙酯和1,3-二(1′,3′-二硫杂-2'-环戊基)丙烷。采用FTIR、1HNMR和GC-MS确定了产品结构。2-iso-butyl-1,3-dithiolane were synthesized by the reaction of 1,2-ethanedithiol with isovaleraldehyde refluxed in benzene, catalyzed by phosphotungstic acid. Effects of mole ratio of 1,2-ethanedithiol to isovaleraldehyde, amount of catalyst and refluxed time were investigated. The optimized reaction conditions were as follows： the mole ratio of 1,2-ethanedithiol and isovaleraldehyde was 1.8, the amount of phosphotungstic acid was 1.7% of the whole reactant, the reaction time was 2.5 h. Four kinds of 1,3-dithiolanes were synthesized under similar condition, which were 2-butyl- 2-methyl-1,3-dithiolane, 1,4-dithiospiro [4.4] nonone, ethyl （2′-methyl-1′ ,3′-dithio-2-cyclopentyl） acetate, and 1,3- di- （1′,3′-dithio-2-cyclopentyl） propane. Structures of five kinds of 1,3-dithiolanes were identified by means of FHR, IH NMR and GC/MS data.

关 键 词：1 3-二硫杂环戊烷 磷钨酸 乙二硫醇 食用香料 合成 

分 类 号：TS264.3[轻工技术与工程—发酵工程]