CAJ | 학술논문

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。
이무이산항위기시원료,통과Grignard、환원화성배반응합성료고순도정위계내지。무이산항화추무완Grignard시제재동염최화하반응득도5-양대계산,질량수솔79.8%;5-양대계산납염경붕경화납환원득도5-간기계산납;최후가염산산화배합득도정위계내지,기상색보분석순도99.6%,질량수솔90%좌우,반응총수솔체72.0%。5-양대계산화정위계내지적결구경IR1、HNMR1、3CNMR화GC-MS표정。
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.