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食用香料糠基2-甲基-3-呋喃基二硫醚的合成
Synthesis of flavor furfuryl 2-methyl-3-furyl disulfide
【摘要】 首先以α-糠基氯和硫代硫酸钠反应制备Bunte盐,然后Bunte盐与2-甲基-3-呋喃硫醇在碱性条件下反应合成了产品糠基2-甲基-3-呋喃基二硫醚。较佳合成工艺为:硫代硫酸钠与α-糠基氯摩尔配比4∶1,氢氧化钠用量8.0 g,反应时间1 h。减压蒸馏后,计算两步反应总产率为31.7%,气相色谱分析糠基2-甲基-3-呋喃基二硫醚相对含量为78.4%。进一步硅胶柱色谱纯化,糠基2-甲基-3-呋喃基二硫醚的结构用质谱、红外光谱、核磁共振进行了确认。
【Abstract】 Bunte salt was first prepared by α-furfuryl chloride and sodium thiosulfate.Then under the reaction of Bunte salt with 2-methyl-3-furanthiol in the presence of sodium hydroxide,furfuryl 2-methyl-3-furyl disulfide was prepared.The optimal synthesis technology was the mole ratio of sodium thiosulfate to α-furfuryl chloride in 4:1,8.0g sodium hydroxide and 1h reaction time.By vacuum distillation,the fraction of furfuryl 2-methyl-3-furyl disulfide was obtained in overall yield of 31.7%,which contained 78.4% furfuryl 2-methyl-3-furyl disulfide in gas chromatography analysis.Further purified by silica gel chromatography,furfuryl 2-methyl-3-furyl disulfide was confirmed by IR,MS and 1H-NMR.
【Key words】 furfuryl 2-methyl-3-furyl disulfide； α-furfuryl chloride； 2-methyl-3-furanthiol； meaty flavor；
- 【文献出处】 食品科技 ,Food Science and Technology , 编辑部邮箱 ,2008年05期
- 【分类号】TQ251.1;TQ655
- 【被引频次】5
- 【下载频次】384