| 丁位癸内酯的合成 |
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| 引用本文： | 赵延伟,贾卫民,王之建,梁立冬.丁位癸内酯的合成[J].上海轻工业高等专科学校学报,2011(2):100-102,107. |
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| 作者姓名： | 赵延伟 贾卫民 王之建 梁立冬 |
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| 作者单位： | 上海应用技术学院香料香精技术与工程学院,上海200235 |
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| 摘 要： | 以戊二酸酐为起始原料,通过Grignard、还原和成环反应合成了高纯度丁位癸内酯。戊二酸酐和溴戊烷Grignard试剂在铜盐催化下反应得到5-氧代癸酸,质量收率79.8%;5-氧代癸酸钠盐经硼氢化钠还原得到5-羟基癸酸钠;最后加盐酸酸化环合得到丁位癸内酯,气相色谱分析纯度99.6%,质量收率90%左右,反应总收率达72.0%。5-氧代癸酸和丁位癸内酯的结构经IR1、HNMR1、3CNMR和GC-MS表征。
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| 关 键 词： | 丁位癸内酯 5-氧代癸酸 戊二酸酐 溴戊烷 硼氢化钠 |
The Synthesis of High Purity 5-Decanolid |
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| ZHAO Yan-wei,JIA Wei-min,WANG Zhi-jian,LIANG Li-dong.The Synthesis of High Purity 5-Decanolid[J].Journal of Shanghai Institute of Technology(Natural Science),2011(2):100-102,107. |
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| Authors: | ZHAO Yan-wei JIA Wei-min WANG Zhi-jian LIANG Li-dong |
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| Affiliation: | (School of Perfume and Aroma Technology,Shanghai Institute of Technology,Shanghai 200235,China) |
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| Abstract: | High purity 5-decanolide was synthesized from glutaric anhydride through grignard reaction,reduction and ring-closure reaction.5-ketocapric acid was prepared from glutaric anhydride and grignard reaqent catalyzed by cupric salt with a yield of 79.8%;5-ketocapric acid was neutralized and subsequently reduced with NaBH4 to afford 5-hydroxydecanoic acid,which was subjected to ring-closure with hydrochloric acid to obtaine 5-decaolide with a yield of 90%.The purity of 5-decanolide was 99.6%.The total yield was 72%.The structures of 5-ketocapric acid and 5-decanolide were characterized by IR,1HNMR,13CNMR and GC-MS. |
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| Keywords: | 5-decanolide 5-ketocapric acid glutaric anhydride 1-bromopentane sodium borohydride |
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