CAJ | 학술논문

以四三苯基膦钯为催化剂，碳酸铯为碱，THF为溶剂，通过脱羧-烷基迁移-芳构化一锅串联反应，将Amorfrutin B合成中的中间体9转化为关环产物10。采用红外光谱、核磁共振氢谱、质谱和元素分析等技术对产物结构进行了表征。通过单因素变量法探讨了钯催化剂用量、碳酸铯用量、反应温度和反应时间对产物产率的影响，得出该反应的最佳工艺条件：物料配比n碳酸铯：n原料=1∶1，钯催化剂为原料9用量的10%，投料温度为0℃，反应温度为室温，反应时间为18h，纯化后产率最高达到53%。
이사삼분기련파위최화제，탄산색위감，THF위용제，통과탈최-완기천이-방구화일과천련반응，장Amorfrutin B합성중적중간체9전화위관배산물10。채용홍외광보、핵자공진경보、질보화원소분석등기술대산물결구진행료표정。통과단인소변량법탐토료파최화제용량、탄산색용량、반응온도화반응시간대산물산솔적영향，득출해반응적최가공예조건：물료배비n탄산색：n원료=1∶1，파최화제위원료9용량적10%，투료온도위0℃，반응온도위실온，반응시간위18h，순화후산솔최고체도53%。
Intermediate 10 for amorfrutin B synthesis was accomplished by a cascade reaction of 9 via a decarboxylation-geranyl migration-cycloaromatization pathway. The structure and purity of the product was characterized by IR, NMR, MS and EA. And the effects of amount of Pd catalyst, amount of Cs2CO3, reaction temperature and reaction time on the reaction yield were also studied. To conclude, the optimized reaction conditions were as followed: 1.0 equivalent Cs2CO3 and 10% equivalent Pd catalyst to starting material 9, reaction temperature 0℃-r. t. and reaction time 18h. The final yield of 10 after purification could reach 53%, which was suitable for industrial process development.