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以对苯二甲醛、丙二腈、季戊四醇和毗咯为原料,合成了含有螺环结构单元的中间体3-[4-(2,2-二氰基)乙烯基]苯基-9-(4-甲酰基)苯基-2,4,8,10-四氧杂螺[5.5]十一烷(3)和α,β,γ,δ-四-(4-甲酰基苯基)卟啉(4).4与过量的季戊四醇反应,得到α,β,γ,δ-四-{4-[2-(5,5-二羟甲基-1,3-二噁烷基)]}苯基卟啉(5),5与3的反应产物经10%NaOH处理后,再与过量的季戊四醇反应,得到α,β,γ,δ-四-{4-[3-(9-(4-(3-(9-(4-(2-(5,5-二羟甲基-1,3-二噁烷基))))苯基一2,4,8,10.四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基]]苯基卟啉(6),6与乙酐、丙酐、苯甲酰氯反应,得到α,β,γ,δ-四-{4-[3-(9-(4-(3-(9-(4-(2-(5,5-二乙酰氧基甲基-1,3-二噁烷基))))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基])苯基卟啉(7),α,β,γ,δ-四-{4-[3-(9-(4-(3-(9-(4-(2-(5,5-二丙酰氧基甲基-1,3-二噁烷基))))苯基.2,4,8,10-四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基]}苯基卟啉(8)和α,β,γ,δ-四-{4-[3-(9-(4-(3-(9-(4-(2-(5,5-二苯甲酰氧基甲基-1,3-二噁烷基))))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基]}苯基卟啉(9)等三种卟啉星形化合物.中间体1~6和星形化合物7~9均进行了IR,1H NMR,MS和元素分析等结构表征.对影响反应的诸因素进行了讨论. 相似文献
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以对苯二甲醛单缩醛与季戊四醇反应得到了2,4,8,10-四氧杂-2,9-二(4-二氰基乙烯基苯基)螺[5.5]十一烷(1), 经水解, 再与丙二腈反应, 制备了中间体2,4,8,10-四氧杂-2-(4-二氰基乙烯基苯基)-9-(4-甲酰基苯基)螺[5.5]十一烷(3). 8-(4-氧代环己烷基)-1,4-二氧杂螺[4.5]癸烷经芳构化形成2,6,10-三-(4-氧代环己烷基)-1,2,3,4,5,6,7,8,9,10,11,12-十二氢苯并[l]菲(4), 再与甲醛进行羟醛缩合, 制成了2,6,10-三-(4-羟基-3,3,5,5-四羟甲基环己烷基)-1,2,3,4,5,6,7,8,9,10,11,12-十二氢苯并[l]菲(5), 将5与过量的3反应, 得到了目标树形大分子化合物2,6,10-三-{15-(3,11-二(-4-(3-((9-(4-二氰基乙烯基)苯基)2,4,8,10-四氧杂螺[5.5]十一烷基)))-7-羟基-二螺[5.1.5.3]十六烷基)}-1,2,3,4,5,6,7,8,9,10,11,12-十二氢苯并[l]菲(6), 收率为18.1%. 产品结构经IR, 1H NMR, MS和元素分析进行了表征. 对影响反应的因素进行讨论. 相似文献
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α,β,γ,δ-四-{4-[3-(9-(4-(3-(9-(4-(2-(5,5-二酰氧基甲基-1,3-二噁烷基))))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5] 十一烷基]}苯基卟啉星形化合物的合成 总被引:1,自引:1,他引:0
以对苯二甲醛、丙二腈、季戊四醇和吡咯为原料, 合成了含有螺环结构单元的中间体3-[4-(2,2-二氰基)乙烯基]苯基-9-(4-甲酰基)苯基-2,4,8,10-四氧杂螺[5.5]十一烷(3)和α,β,γ,δ-四-(4-甲酰基苯基)卟啉(4). 4与过量的季戊四醇反应, 得到α,β,γ,δ-四-{4-[2-(5,5-二羟甲基-1,3-二噁烷基)]}苯基卟啉(5), 5与3的反应产物经10% NaOH 处理后, 再与过量的季戊四醇反应, 得到α,β,γ,δ-四-{4-[3-(9-(4-(3-(9-(4-(2-(5,5-二羟甲基-1,3-二噁烷基))))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基]}苯基卟啉(6), 6与乙酐、丙酐、苯甲酰氯反应, 得到α,β,γ,δ-四-{4-[3-(9-(4-(3- (9-(4-(2-(5,5-二乙酰氧基甲基-1,3-二噁烷基))))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基]}苯基卟啉(7), α,β,γ,δ-四-{4-[3-(9-(4-(3-(9-(4-(2-(5,5-二丙酰氧基甲基-1,3-二噁烷基))))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基]}苯基卟啉(8)和α,β,γ,δ-四-{4-[3-(9-(4-(3-(9-(4-(2-(5,5-二苯甲酰氧基甲基-1,3-二噁烷基))))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基)))苯基-2,4,8,10-四氧杂螺[5.5]十一烷基]}苯基卟啉(9)等三种卟啉星形化合物. 中间体1~6和星形化合物7~9均进行了IR, 1H NMR, MS和元素分析等结构表征. 对影响反应的诸因素进行了讨论. 相似文献
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本实验采用季戊四醇与苯三甲醛缩合, 制成树状化合物1,3,5-三{3-|[2,4,8,10-四氧杂-9(3,5-二(2,6-二氧杂-4,4-二羟甲基环己基)苯基)螺[5.5]十一烷基}苯. 该类树状分子具有手性螺环结构, 手性密度很高, 可开发成理想的高效手性催化剂[3~8], 具有诱人的应用前景. 相似文献
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聚缩醛螺胞二醚的合成及结构表征 总被引:3,自引:0,他引:3
在I2催化剂的作用下, 利用苯甲醛与季戊四醇反应, 制备了聚缩醛螺胞二醚的模型化合物3,9-二苯基-2,4,8,10-四氧杂螺[5.5]十一烷(1). 在此基础上, 利用1,3-苯二甲醛与不同摩尔比的季戊四醇合成了化合物1,3-二(2,6-二氧杂-4,4-二羟甲基环己基)苯(2)和2,4,8,10-四氧杂-3,9-二(3'-甲酰基苯基)螺[5.5]十一烷(3). 化合物2与化合物3反应, 制成标题化合物聚缩醛螺胞二醚4, 收率为95.4%. 用FTIR, 1H NMR对化合物1~4的结构进行了表征. 发现在含有手性轴化合物1, 3, 4的1H NMR谱中, 4个亚甲基中的8个氢原子裂分为4组双峰, 而不含有手性轴化合物中的4个亚甲基中的8个氢原子不裂分, 是个单峰. 这种不同不是由于化合物中刚性环所致, 而是由于有无手性轴造成的. 相似文献
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以取代苯酚4和对氟苯乙酮(5)为原料,经4步反应合成关键中间体1-(4-取代苯氧苯基)乙胺(9),再与3种中间体2-氰基-3-乙氧基-2-戊烯酸乙氧乙酯(1)、2-氰基-3,3-二甲硫基丙烯酸乙氧乙酯(2)和2-氰基-3-氯-4,4,4-三氟丁烯酸乙氧乙酯(3)分别发生缩合反应,合成了3个系列共35个新2-氰基-3-[1-(4-取代苯氧基苯基)乙胺基]烯酸乙氧乙酯类化合物(10,11和12).所有新化合物的结构均经过1H NMR,13C NMR,19F NMR和HRMS的确证,并测试了目标化合物的除草活性,部分化合物在剂量为93.75 g/ha时,对双子叶植物油菜和苋菜的抑制率为100%. 相似文献
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报道了"一锅法"合成含两种桥联链的新型杯[4]双冠醚和双杯[4]冠醚.杯[4]芳烃先与N,N’-乙撑基-二(2-氯乙酰胺)发生"1+1"缩合反应,然后直接加入三甘醇双对甲苯磺酸酯继续进行"2+2"缩合反应,合成了含两种桥联链的新型双杯[4]冠醚4.按照相似程序,杯[4]芳烃先后与N,N’-乙撑基-二(2-氯乙酰胺)、溴乙酸乙酯和二乙烯三胺反应,得到含两种桥联链的新型杯[4]双冠醚5.化合物5进一步与异硫氰酸苯酯反应合成带硫脲支链的杯[4]双冠醚6.所有新化合物的结构与构象经元素分析、质谱、核磁共振谱等表征证实. 相似文献
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Wetherby AE Goeller LR DiPasquale AG Rheingold AL Weinert CS 《Inorganic chemistry》2007,46(18):7579-7586
The protonolysis reaction of the germanium(II) amide Ge[N(SiMe3)2]2 with calix[4]arene and calix[8]arene furnishes the two germanium(II) calixarene complexes {calix[4]}Ge2 and {calix[8]}Ge4, respectively, which have been crystallographically characterized. The calix[4]arene complex contains a Ge2O2 rhombus at the center of the molecule and is one of the only four germanium(II) calix[4]arenes that have been structurally characterized. The calix[8]arene species is the first reported germanium calix[8]arene complex, and it exhibits an overall bowl-shaped structure which contains two Ge2O2 fragments. The latter complex reacts with Fe2(CO)9 to yield an octairon compound, which has also been structurally characterized and contains four GeFe2 triangles arranged around the macrocyclic ring. The germanium(II) centers are oxidized to germanium(IV) in this process, with concomitant reduction of the neutral diiron species to Fe2(CO)(8)2- anions. 相似文献
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Salmon L Thuéry P Ephritikhine M 《Dalton transactions (Cambridge, England : 2003)》2006,(30):3629-3637
Reactions of UCl4 with calix[n]arenes (n = 4, 6) in THF gave the mononuclear [UCl2(calix[4]arene - 2H)(THF)2].2THF (.2THF) and the bis-dinuclear [U2Cl2(calix[6]arene - 6H)(THF)3]2.6THF (.6THF) complexes, respectively, while the mono-, di- and trinuclear compounds [Hpy]2[UCl3(calix[4]arene - 3H)].py (.py), [Hpy](4)[U2Cl6(calix[6]arene - 6H)].3py (.3py), [Hpy]3[U2Cl5(calix[6]arene - 6H)(py)].py (.py) and [Hpy]6[U3Cl11(calix[8]arene - 7H)].3py (.3py) were obtained by treatment of UCl4 with calix[n]arenes (n = 4, 6, 8) in pyridine. The sodium salt of calix[8]arene reacted with UCl4 to give the pentanuclear complex [U{U2Cl3(calix[8]arene - 7H)(py)5}2].8py (.8py). Reaction of U(acac)4 (acac = MeCOCHCOMe) with calix[4]arene in pyridine afforded the mononuclear complex [U(acac)2(calix[4]arene - 2H)].4py (.4py) and its treatment with the sodium salt of calix[8]arene led to the formation of the 1D polymer [U2(acac)6(calix[8]arene - 6H)(py)4Na4]n. The sandwich complex [Hpy]2[U(calix[4]arene - 3H)2][OTf].4py (.4py) was obtained by treatment of U(OTf)4 (OTf = OSO2CF3) with calix[4]arene in pyridine. All the complexes have been characterized by X-ray diffraction analysis. 相似文献
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Fafu Yang Xiaohua Zheng Hongyu Guo Zhaohui Liu Yu Guo 《Journal of inclusion phenomena and macrocyclic chemistry》2008,62(3-4):371-375
By reacting calix[4]-1,3-aza-crown 2 with 1,6-diisocyanatohexane in “1+2” condensation mode, the first example dumbbell shaped biscalix[4]-1,3-aza-crown 3 was conveniently prepared in yield of 94%. The complexation properties of compound 3 were investigated by UV–vis spectra and 1H NMR experiments. The results showed that compound 3 has good complexation abilities for anions. Compound 3 binded monoacidic anions with 1:2 binding-stoichiometry and binded binary acidic anions with 1:1 binding-stoichiometry. 相似文献