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第 43 卷第 5 期Vol. 43 No. 5
2013 年 10 月Oct 2013

所屬欄目:醫藥及中間體

雙聯(lián)芐類(lèi)化合物中間體二苯醚類(lèi)化合物的合成及表征
劉德秀,潘華英 (蘇州衛生職業(yè)技術(shù)學(xué)院, 江蘇 蘇州 215009)
摘 要:以酚類(lèi)化合物和鹵代芳香醛或鹵代芳香酯類(lèi)化合物為原料,通過(guò)醛保護和Ullmann反應合成系列二苯醚類(lèi)化合物?疾榱舜呋瘎、縮合劑和混合縮合劑的比例對反應收率的影響,結果表明,當催化劑為氧化銅、縮合劑為混合碳酸鈣和碳酸鉀,投料比為n(酚類(lèi)化合物)∶n(鹵代化合物)∶n(氧化銅)∶n(碳酸鉀)∶n(碳酸鈣)=1∶1.05∶0.3∶1.6∶0.4,收率較理想。目標產(chǎn)物的結構通過(guò)MS和1H NMR確證。
關(guān)鍵詞:合成;醛保護;二苯醚;Ullmann反應
中圖分類(lèi)號:0625  文獻標識碼:A  文章編號:1009-9212(2013)05-0038-04
Synthesis and Characterization of Diphenyl Ethers - Intermediates for Bisbibenzyl Compounds
LIU De-xiu,PAN Hua-ying (Suzhou Health College,Suzhou 215009,China)
Abstract:Diphenyl ethers were important intermediates for synthesizing bisbibenzyl compounds. In this paper,diphenyl ethers were synthesized from phenolic compound and halogenated aromatic aldehydes or halogenated aromatic esters. The reaction conditions affecting the yield,such as catalyst,condensing agents and mixed condensing agents had been screened. It was found that cupric oxide and the mixture of calcium carbonate with potassium carbonate was the best catalyst and condensing agent,respectively. The optimum ratio of raw materials was proved as follows:n(phenolic compound)∶n(halogenated compound)∶n(cupric oxide)∶n(potassium carbonate)∶n (calcium carbonate)= 1∶1.05∶0.3∶1.6∶0.4. The product structures were confirmed with MS and 1H NMR.
Key words:synthesis;protection of the aldehyde;diphenyl ether;Ullmann reaction
作者簡(jiǎn)介:劉德秀(1966-),女,江蘇建湖人,副教授,碩士,研究方向:主要從事藥物合成和教育教學(xué)研究。(E-mail:dxliu@szhct.edu.cn)
收稿日期: 2013-09-1
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