CAJ | 학술논문

目的：探讨影响苯酞开环反应的因素和优化反应条件。方法以乙醇钠与对羟基苯乙酸为原料合成亲核试剂二钠盐，其进攻苯酞发生开环反应。考察合成亲核试剂所用碱、苯酞加料方式、反应溶剂及温度的影响。结果以乙醇钠作碱，分步加料，DMAC作溶剂，166℃回流条件下反应3 h，产率达78％以上，结构经1 H-NMR确认。结论在优化条件下，缩短了反应时间，提高了产率。同时，根据实验结果，推断出了苯酞的开环位置和可能的开环机理。
목적：탐토영향분태개배반응적인소화우화반응조건。방법이을순납여대간기분을산위원료합성친핵시제이납염，기진공분태발생개배반응。고찰합성친핵시제소용감、분태가료방식、반응용제급온도적영향。결과이을순납작감，분보가료，DMAC작용제，166℃회류조건하반응3 h，산솔체78％이상，결구경1 H-NMR학인。결론재우화조건하，축단료반응시간，제고료산솔。동시，근거실험결과，추단출료분태적개배위치화가능적개배궤리。
Objective To study the influencing factors of the ring opening reaction of phthalide and op-timize the reaction conditions. Methods Disodium salt was synthesized by sodium ethoxide and 4-hydroxyphenyl acetic acid as a nucleophilic reagent,which attacks phthalide to make it ring opened.The influencing factors of the reaction,such as alkali,material feeding of phthalide,solvent and temperature were studied.Results With sodium ethoxide as alkali,multistep feeding,DMAC as a solvent and reflu-xing at 166 ℃ for 3 h,the yield was increased to 78% or more,the structure was characterized by 1H-NMR. Conclusion Under the optimal conditions,the reaction time could be shortened,the yield could be raised.At the same time,the opening position and its mechanism might be inferred,according to the experimental results.