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以N-苯基-1-萘胺和对溴碘苯为起始原料,经Buchwald-Hartwing偶联反应合成有机发光二极管空穴传输材料N,N′-二[4-(1-萘基苯基氨基)苯基]-N,N′-二苯基-[1,1′-联苯]-4,4′-二胺(2)。以1-溴化萘(1-溴萘)为初始原料与N,N′-二苯基联苯二胺经Buchwald-Hartwing偶联合成了N,N′-[二(1-萘基)-N,N′-二苯基]-1,1′-联苯基)-4,4′-二胺(NPB)。利用~1HNMR、LC-MS等对产品结构进行表征。通过差示扫描量热仪(DSC)测得化合物2和NPB失重5%的温度分别为510℃和491℃,化合物2的玻璃化转变温度Tg为126℃,化合物2和NPB的升华温度分别为395℃和290℃,并通过UV-Vis紫外吸收光谱、荧光光谱研究了两种传输材料的光学性质。 相似文献
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以2-萘酚和80%水合肼为起始原料,经3步反应生成光学活性的2,2’-二胺-1,1’-联萘,该对映体再依次经过溴代、锂化及羧基化反应制备得到了手性1,1’-联萘-2,2’-二甲酸,收率为68.4%(以2,2’-二溴-1,1’-联萘计),光学纯度为84%。各步产物的结构经1H NMR、13C NMR得到确证。该反应原料价廉易得,整个操作过程简单安全,具有一定的应用研究价值。 相似文献
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重氮化法(用胺盐形式)制备偶氮萘 总被引:1,自引:0,他引:1
2,2′—偶氮萘为一种重要的抗氧剂和光敏剂,并且经还原、重排得2,2′—二氨基1,1′—联萘,该化合物是研究立体活性染料及轴不对称合成的重要试剂。如以β—萘胺为原料,经重氮化、Na_2SO_3还原得偶氮萘。但由于β—萘胺在盐酸—硫酸体系中的水溶性甚差,按文献报导方法仅得10%产率。我们改用胺盐形式 相似文献
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1,4二-氢-3H-2,3苯-并口恶嗪-3甲-酸乙酯经过硝化、还原和重氮化溴代得到了7溴--1,4二-氢-3H-2,3苯-并口恶嗪-3甲-酸乙酯(C)。以Pd(OAc)2/R(+)B INAP(2,2′-二苯膦-1,1′-联萘)为催化体系,C与苯胺、N-甲基苯胺、对氟苯胺、对乙氧基苯胺、环己胺、吗啡、四氢吡咯及六氢吡啶等8种有机胺类化合物(Am ine1~8),在氮气保护下,以碳酸铯为碱于干燥的甲苯中100℃反应16~24 h,生成了相应的8种新的7胺-基取代的1,4二-氢-3H-2,3苯-并口恶嗪-3甲-酸乙酯类化合物(D1~8),反应收率分别为83%、85%、71%、90%、72%、63%、75%和83%。通过1HNMR、质谱和元素分析对这些化合物的结构进行了表征。 相似文献
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以2-氰基吡啶和水合肼为原料,经过Pinner反应和氧化反应合成得到3,6-二(吡啶-2-基)-1,2,4,5-四嗪(化合物1),收率为88.6%。对影响产物收率的因素进行了考察,确定了第二步氧化反应的反应温度为0℃,反应时间1.0h。化合物1分别与6,7-二溴-1,4-二氢-1,4-环氧萘(化合物4a)和6,7-二甲氧基-1,4-二氢-1,4-环氧萘(化合物4b)反应得到5,6-二溴异苯并呋喃(化合物5a)和5,6-二甲氧基异苯并呋喃(化合物5b)的收率分别为51.3%和48.5%。化合物1和化合物5a以及化合物5b的结构均采用~1H-NMR和ESI-MS进行了表征。 相似文献
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Studies on Stereoselective Electrophiic Cyanation The enantioselective, electrophilic cyanation of the enolates of 2-substituted 1-tetralones 3 is described. Enantiomerically pure 2-cyanato-1,1′-binaphthyl derivatives 2, 6a and b are used as cyanating agents. The influence of solvent, temperature, additives and the method of enolate formation are investigated. Best results are obtained with 48% ee in the case of compound 2 and 60% ee in the case of compound 6b if the enolate is prepared from the corresponding silyl enol ether 7 and Toluene is used as solvent. 相似文献
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Henry C. Duffin Peter Golding Clifford H. J. Wells 《Propellants, Explosives, Pyrotechnics》1998,23(5):244-245
Conditions for the synthesis of 4,4′,5,5′,7,7′-hexanitrobinaphthyl( I ) from 1,1′-binaphthyl have been investigated. It has been found that( I ) can be prepared in 50% yield in a two-stage nitration process. 相似文献
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Yehui Chen Liwen Yang Nianfa Yang Jingyi Yan Zhusheng Yang Jian Zhang 《Polymer Bulletin》2014,71(10):2507-2521
The synthesis and chiroptical properties of a novel optically active helical polymers, poly[(S)-6-acryloyl-2,2′-bisalkoxy-1,1′-binaphthyl] (poly-3), were reported. All the monomers readily underwent anionic polymerization to yield the polymers displaying optical rotations and Cotton effects in the UV–vis absorption region of side groups distinct to monomers (3) and the corresponding model compounds such as (S)-6-propionyl-2,2′-bisalkoxy-1,1′-binaphthyl (4) and (S)-6-heptanoyl-2,2′-bisalkoxy-1,1′-binaphthyl (5), implying the formation of main-chain chirality, most probable helicity. Their helical conformations were quite stable as revealed by the almost unchanged chiroptical properties measured at different temperatures. 相似文献
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The two symmetric binaphthyls (1,1″- and 2,2″-binaphthyl) were synthesized by Grignard coupling reactions of 1-bromonaphthalene and 2-bromonaphthalene, respectively, using two different promoters (Ni(acac)2 and 1,4-dichloro-2-butene). The non-symmetric 1,2″-binaphthyl was prepared via two methods: (1) coupling of 2-naphthylmagnesium bromide with 1-tetralone, followed by dehydration, then sulfur-catalyzed dehydrogenation and (2) a Kharash-type Grignard coupling between 1-naphthylmagnesium bromide and 2-bromonaphthalene, with Ni(acac)2 as the promoter. The binaphthyls were exposed to room-and high-temperature tetrachloroaluminate molten salts of differing composition. 1,1″-Binaphthyl and 1,2″-binaphthyl isomerized to 2,2″-binaphthyl in the room temperature molten salts, whereas 2,2″-binaphthyl was unchanged. In molten salts at temperatures in excess of 75?, each of the binaphthyls underwent cyclodehydrogenation to form perylene and small amounts of benzofluoranthenes. 相似文献
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报道了以具有抗癌和抗艾滋病毒活性的β-D-氨基葡萄糖与二茂铁二甲酸作起始原料合成一种糖/金属有机化合物——N,N′-二茂铁二甲酰氨基葡萄糖的方法。第一步,将氨基葡萄糖用苯甲醛保护氨基后,用乙酸酐再保护羟基,然后在加有盐酸的丙酮中去氨基保护,得1,3,4,6-四-O-乙酰基-β-D-氨基葡萄糖盐酸盐;将二茂铁二甲酸与草酰氯在干燥的二氯甲烷中反应得到二茂铁二甲酰氯。第二步,将第一步所得的两个中间产物,在室温下加入干燥的二氯甲烷和苯的混合溶剂中,在三乙胺存在下进行反应,得目标产物,收率35.7%,系红棕色固体,熔点198~200℃。目标化合物是具有双药效基团的物质。用元素分析,红外光谱和核磁共振波谱进行了表征。 相似文献
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Li Xiang Furen Zhang Jiaxin Zhang Haibin Song Guofu Zi 《Inorganic chemistry communications》2010,13(5):666-670
Five group 4 metal complexes (1)2Zr(NMe2)2 (5), (2)2Ti(NMe2)2 (6), (2)2Zr(NMe2)2 (7), (3)2Zr (8) and (4)2Ti(NMe2)2 (9) have been readily prepared from the reaction between M(NMe2)4 (M = Ti, Zr) and chiral binaphthyldiamine-based ligands, (R)-2,2′-bis(diphenylthiophosphoramino)-1,1′-binaphthyl (1H2), (R)-5,5′,6,6′,7,7′,8,8′-octahydro-2,2′-bis(diphenylthiophosphoramino)-1,1′-binaphthyl (2H2), (R)-5,5′,6,6′,7,7′,8,8′-octahydro-2,2′-bis(methanesulphonylamino)-1,1′-binaphthyl (3H2), and C1-symmetric ligand, (R)-2-(mesitylenesulphonylamino)-2′-(dimethylamino)-1,1′-binaphthyl (4H). All the complexes have been characterized by various spectroscopic techniques, elemental analyses and X-ray diffraction analyses. The zirconium amides are active catalysts for the asymmetric hydroamination/cyclization of aminoalkenes, affording cyclic amines in good yields with moderate ee (enantiomeric excess) values. 相似文献
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Min Mo Tao Yi Cong-Ye Zheng Mao-Lin Yuan Hai-Yan Fu Rui-Xiang Li Hua Chen 《Catalysis Letters》2012,142(2):238-242