4-异丁酰氧基-2-环庚烯-1-酮的合成研究

Synthesis of 4-Isobutyrate-2-Cyclohepten-1-One

通过异丁酰氯和4-羟基-2-环庚烯-1-酮缩合制备了4-异丁酰氧基-2-环庚烯-1-酮。在无缩合剂的条件下,考察了4-二甲氨基吡啶(DMAP)的物质的量、反应温度、反应时间等对酯化反应的影响。结果表明,该反应较佳的DMAP的物质的量为0.3 mmol,较佳温度为25℃,较佳的反应时间为3 h;在以上反应条件下,酯化产物的产率为89%。核磁表征结果表明,合成的产物为目标产物4-异丁酰氧基-2-环庚烯-1-酮。该反应条件温和,无需缩合剂参与,产率高,符合绿色化学发展的概念。

4-Isobutyloxy-2-cyclohepten-1-one was prepared by the condensation of isobutyryl chloride and 4-hydroxy-2-cyclohepten-1-one.The effects of various amounts of 4-dimethylaminopyridine(DMAP),reaction temperature and reaction time on the esterification reaction were investigated under the condition of no condensation agent.The results show that the optimized reaction condition is 0.3 mmol of DMAP under 25℃for 3 h with a yield of 89%.The results of the NMR show that the synthesized product was the target molecule 4-isobutyloxy-2-cyclohepten-1-one.This esterification reaction features high yields under mild reaction conditions without the involvement of condensation agents,which is in line with the concept of the development of green chemistry.