【摘要】 分别以吡啶和三乙胺为催化剂,在传统加热和微波辐射两种条件下对5种目标产物进行了合成,其中目标产物Ⅱ、Ⅳ和Ⅴ经科技查新证实均属国内外文献未公开报道的新型化合物,其新颖性已为教育部科技查新工作站(吉林大学查新检索咨询中心)的200604311212号《科技查新报告》所证实。以吡啶为催化剂,目标产物产率由传统加热下的61.6%提高到微波辐射下的81.6%,反应时间缩短为传统的1/100;以三乙胺为催化剂,目标产物产率由传统加热下的75.2%提高到微波辐射下的94.4%,反应时间缩短为传统的1/15。通过元素分析、MS谱、1HNMR谱对所合成的目标产物分别进行了全面的表征,证实了其分子结构。并对5种目标产物进行了紫外测试,得出其最大吸收峰在315 nm左右。实验结果表明:当糠偶姻的用量为20 mmol时,最适宜反应条件为:n(糠偶姻)∶n(酰氯)=1∶2.2,有机碱三乙胺的用量为25 mL,微波工作功率为240 W,辐射时间10 min,产率94%以上。更多还原

【Abstract】 The target products were synthesized in the presence of pyridine and triethylamine as catalysts under traditional calefaction and microwave irradiation.With pyridine as catalyst,the yield was raised from 61.6%(under traditional calefaction) to 81.6%(under microwave irradiation),and the reaction time was decreased to 1/100 times.With triethylamine as catalyst,the yields raised from 75.2%(under traditional calefaction) to 94.4%(under microwave irradiation),and the reaction time was decreased to 1/15 times.By characterization with elementary analysis,MS and 1HNMR,the structural formula of 5 target products were distinctively demonstrated.Their max.UV absorbance were near 315 nm.The experimental results show the best synthesis conditions:furoin 20 mmol,n(furoin)∶n(acid chloride)=1∶2.2,triethylanine 25 mL,power of microwave 240 W and radiation time 10 min.Yields of the products were over 94%.更多还原