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本文以N-(3-溴丙基)邻苯二甲酰亚胺合成为模板反应,研究了相转移催化无溶剂合成N-(ω-溴烷基)邻苯二甲酰亚胺的影响因素,实验证实相转移催化剂及其用量、催化剂K2CO3的用量等对反应的影响明显,得到N-(3-溴丙基)邻苯二甲酰亚胺的优化合成条件为:反应物配比为PA∶C3Br2∶K2CO3∶TBAB=1∶2∶4∶0.2,反应温度80℃,反应时间1h,N-(3-溴丙基)邻苯二甲酰亚胺产率为92%。在相同反应条件下,N-(ω-溴烷基)邻苯二甲酰亚胺的产率随α,ω-二溴烷烃的烷基链长度增加而降低。 相似文献
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本文报道合成N-(苯基·乙亚基)苯甲胺的二碳负离子的新方法。经多方实验,只有用N-(苯基·乙亚基)苯甲胺与一当量的正丁基锂和二异丙基胺锂反应得到1,4-二碳负离子,硅烷化得到1,4-二硅烷基衍生物。 相似文献
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《合成化学》2015,(9)
以1-金刚烷甲酸为原料,经酰化,取代和还原反应制得N,N-二甲基-1-金刚烷基甲胺(1);1与双子季铵盐(2)在无水乙醇中反应合成了一种新型的金刚烷基杂双子表面活性剂——1-(N,N-二甲基-1-金刚烷甲基溴化铵)-6-(N,N-二甲基-十二烷基溴化铵)-己烷(3),总收率30.9%,其结构经1H NMR和元素分析表征。采用表面张力法研究了3的表面活性。结果表明:3具有较强的聚集能力和界面吸附能力,其cmc,γcmc,p C20,Γmax,Amin分别为1.18 mmol·L-1,35.5 m N·m-1,0.48,2.63μmol·m-2和0.63 nm2。 相似文献
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金刚烷基甜菜碱型和季铵盐阳离子型表面活性剂的合成研究 总被引:1,自引:0,他引:1
以金刚烷胺为起始反应物,首先在过量甲酸存在下,与甲醛发生埃斯韦勒-克拉克甲基化反应合成了N,N-二甲基金刚烷叔胺,在此基础上通过N,N-二甲基金刚烷叔胺与氯乙酸钠、溴代正丁烷、溴代正辛烷、溴代十二烷、溴代十六烷等一系列季铵化试剂的季铵化反应,分别合成了N,N-二甲基金刚烷甜菜碱型表面活性剂及N-(1-金刚烷基)-N,N-二甲基正丁基溴化铵、N-(1-金刚烷基)-N,N-二甲基辛基溴化铵、N-(1-金刚烷基)-N,N-二甲基十二烷基溴化铵、N-(1-金刚烷基)-N,N-二甲基十六烷基溴化铵等金刚烷季铵盐阳离子型表面活性剂,产率分别为75%,75%,61%,44%,54%.采用元素分析,IR,1H NMR等分析手段对5种产物进行了结构鉴定,测试了各种金刚烷表面活性剂水溶液的表面张力. 相似文献
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本文报告某些N,N-双取代氨甲基膦酸酯及其衍生物的红外光谱的研究.N,N-双取代氨甲基膦酸一烷基酯在2500厘米~(-1)左右显示宽广的NH吸收,在1210-1230厘米~(-1)及1060-1090厘米~(-1)分别显示POO~-不对称及对称吸收,其钠盐在2500厘米~(-1)左右无吸收,而在1200-1225厘米~(-1)及1060-1080厘米~(-1)也分别显示POO~-不对称及对称吸收,这些结果表明N,N-双取代氨甲基膦酸一烷基酯是以两性离子存在.N,N-双取代氨甲基膦酸二烷基酯及一烷基酯可用纸层析和纸电泳分离并讨论取代烷基及酯烷基与比移值及泳动度的关系. 相似文献
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β-(3,4-二甲氧基)苯乙胺与甲醛及甲酸在封管中热至125°,生成N,N-二甲基衍生物.2-溴-1-(3,4-二甲氧基)苯乙烷与二乙胺或六氢吡啶缩合则成相应N,N-二乙基衍生物或N-六氢吡啶衍生物.在无水碳酸钠作用下,N-甲基-β-(3,4-二甲氧基)苯乙胺经氯化苄、2-溴-1-苯乙烷或2-溴-1-(3,4-二甲氧基)苯乙烷烷化,分别生成相应N-甲基-N-芳烷基-β-(3,4-二甲氧基)苯乙胺.β-(3,4-二甲氧基)苯乙胺经乙酸酐或苯乙酰氯酰化后,再以五氧化二磷环化,并以锌粉及盐酸还原,分别制成1-甲基及1-苄基-6,7-二甲氧基-1,2,3,4-四氢异喹啉.以上制成的化合物均可认为是镇痛药延胡索素乙的裂环化合物,并已进行药理试验. 相似文献
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Synthesis and antitumor properties of N1-acyloxymethyl derivatives of bis(2,6-dioxopiperazines) 总被引:1,自引:0,他引:1
J C Cai H L Shu C F Tang T Komatsu T Matsuno T Narita S Yaguchi Y Koide M Takase 《Chemical & pharmaceutical bulletin》1989,37(11):2976-2983
Many N1-acyloxymethyl derivatives VI of bis(2,6-dioxopiperazine) I, ICRF-154, were prepared and tested for antitumor activity. The treatment of I with formaldehyde gave a crystalline bis(N1-hydroxymethyl) derivative VII, which was acylated under various conditions to give bis(N1-acyloxymethyl) derivatives VI. Antitumor activity of VI against P388 leukemia in mice was studied. Several bis(N1-acyloxymethyl) compounds such as phenylacetyloxymethyl VI-6, methoxycarbonyloxymethyl VI-41, isobutoxycarbonyloxymethyl VI-44, and furancarboxymethyl VI-38 compounds were found to have potent antitumor activities. On the other hand, water-soluble esters having an amine or a carboxylic acid function in their acyl groups showed rather reduced activity. These bis(N1-acyloxymethyl) derivatives VI were presumably hydrolyzed into the parent bis(2,6-dioxopiperazine) I by nonspecific esterase in the body to exhibit their antitumor activity. 相似文献
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[9-[10-(4-t-Butyl-2,6-dimethyl)phenyl]anthryl](4-bromo-2,6-dimethylphenyl)diazomethane (1-N(2)) was found to be stable enough to survive under Sonogashira and Suzuki coupling reaction conditions, and bis(diazo) compounds incorporated into the 1,4-positions of butadiyne (3-2N(2)) and the 2,5-position of thiophene (4-2N(2)) were prepared. Irradiation of those bis(diazo) compounds generated bis(carbenes), which were characterized by ESR and UV-vis spectroscopic techniques in a matrix at low temperature, as well as time-resolved UV-vis spectroscopy in solution at room temperature. These studies revealed that both of the bis(carbenes), 3 and 4, have a singlet quinoidal diradical ground state with a very small singlet-triplet energy gap of less than 1 kcal/mol. A remarkable increase in the lifetime of bis(carbenes) as opposed to that of monocarbene (1) was noted and was interpreted to indicate that bis(carbenes) are thermodynamically stabilized as a result of delocalization of unpaired electrons throughout a pi-net framework. Despite the stability, both bis(carbenes) are readily trapped by molecular oxygen to afford bis(ketones) as main products. 相似文献
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A new type of 1D infinite inorganic [n]catenane framework was self-assembled by silver nitrate and bis(2-methylimidazolyl)methane, while a comparatively one-dimensional zigzag cationic chain was generated by AgNO(3) and bis(imidazol-1-yl)methane. 相似文献
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Holschumacher D Hrib CG Jones PG Tamm M 《Chemical communications (Cambridge, England)》2007,(35):3661-3663
The chiral carbene bis[bis(R-1-phenylethyl)amino]cyclopropenylidene 2 and its dicarbene-silver complex [Ag(2)2]BF4 (3) have been isolated in good yields from the reactions of bis[bis(R-1-phenylethyl)amino]cyclopropenylium tetrafluoroborate (1)BF4 with potassium bis(trimethylsilyl)amide or with Ag2O, respectively; the molecular structures of (1)ClO4, 2 and 3 have been determined by X-ray diffraction analyses. 相似文献
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Gerd Becker Mark Niemeyer Otto Mundt Wolfgang Schwarz Matthias Westerhausen Manfred W. Ossberger Peter Mayer Heinrich Nth Zhiyuan Zhong Pieter J. Dijkstra Jan Feijen 《无机化学与普通化学杂志》2004,630(15):2605-2621
Crystal Structures and Spectroscopic Properties of 2λ3‐Phospha‐1, 3‐dionates and 1, 3‐Dionates of Calcium ‐ Comparative Studies on the 1, 3‐Diphenyl and 1, 3‐Di(tert‐butyl) Derivatives A hydrogen‐metal exchange between dibenzoylphosphane and calcium carbide in tetrahydrofuran (THF) followed by addition of the ligand 1, 3, 5‐trimethyl‐1, 3, 5‐triazinane (TMTA) furnishes the binuclear complex bis[(tmta‐N, N′, N″)calcium bis(dibenzoylphosphanide)] ( 1a ) co‐crystallizing with benzene. Similarly, reaction of bis(2, 2‐dimethylpropionyl)phosphane with bis(thf‐O)calcium bis[bis(trimethylsilyl)amide] in 1, 2‐dimethoxyethane (DME) gives bis(dme‐O, O′)calcium bis[bis(2, 2‐dimethylpropionyl)phosphanide] ( 1b ) in high yield. The carbon analogues 1, 3‐diphenylpropane‐1, 3‐dione (dibenzoylmethane) or 2, 2, 6, 6‐tetramethylheptane‐3, 5‐dione (dipivaloylmethane) and bis(thf‐O)calcium bis[tris(trimethylsilylmethyl)zincate] in DME afford bis(dme‐O, O′)calcium bis(dibenzoylmethanide) ( 2a ) and the binuclear complex (μ‐dme‐O, O′)bis[(dme‐O, O′)calcium bis(dipivaloylmethanide)] ( 2b ), respectively. Dialkylzinc formed during the metalation reaction shows no reactivity towards the 1, 3‐dionates 2a and 2b . Finally, from the reaction of the unsymmetrically substituted ligand 2‐(methoxycarbonyl)cyclopentanone and bis(thf‐O)calcium bis[bis(trimethylsilyl)amide] in toluene, the trinuclear complex 3 is obtained, co‐crystallizing with THF. The β‐ketoester anion bridges solely via the cyclopentanone unit. 相似文献
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A series of novel bis(beta-cyclodextrin)s tethered with organoselenium linkers, i.e., 6,6'-(o-phenylene-diseleno)-bridged bis(beta-cyclodextrin) (2), 6,6'-[2,2'-diselenobis(benzoyloxy)]-bridged bis(beta-cyclodextrin) (3), and 6,6'-[2,2'-diselenobis[2-(benzoylamino)ethylamino]]-bridged bis(beta-cyclodextrin) (4), were synthesized from beta-cyclodextrin (1). The inclusion complexation behavior of 1-4 with some dyes, such as 8-anilinonaphthalenesulfonate (ANS), Brilliant Green, Crystal Violet, Tropaeolin OO, Auramine O, and Methyl Orange, was investigated in aqueous phosphate buffer solution (pH 7.20) at 25 degrees C by UV-vis, fluorescence, and circular dichroism spectrometry, as well as fluorescence lifetime measurements. The complex stability constants (Ks) and Gibbs free energy changes (delta Go) for the stoichiometric 1:1 inclusion complexation of 1-4 with the dyes were obtained by the spectrophotometric or spectropolarimetric titrations. The bis(beta-cyclodextrin)s 2-4 showed much higher affinities toward these guest dyes than native beta-cyclodextrin 1 with fairly good molecular selectivities. The cooperative binding abilities of these bis(beta-cyclodextrin)s are discussed from the viewpoints of size/shape-fit interaction, induced-fit concept, and multiple recognition mechanism. 相似文献
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(2,6-dimethyl-4-tert-butylphenyl)(2,4,6-tribromophenyl)diazomethane(-N(2)) was found to be stable enough to survive under Sonogashira coupling reaction conditions, and aryldiazomethyl substituents were introduced at the 1,4-positions of butadiyne (4-2N(2)) and the 2,5-positions of thiophene(5-2N(2)). Irradiation of those bis(diazo) compounds generated bis(carbenes), which were characterized by using ESR and UV/vis spectroscopic techniques in a matrix at low temperature as well as time-resolved UV/vis spectroscopy in solution at room temperature. These studies revealed that both of the bis(carbenes), 4 and 5, have singlet quinoidal diradical ground states with a very small singlet-triplet energy gap of less than 1 kcal mol(-1). A remarkable increase in the lifetime of bis(carbenes), as opposed to that of the monocarbene (2), was noted and was interpreted to indicate that bis(carbenes) are thermodynamically stabilized as a result of delocalization of unpaired electrons throughout the pi net framework. In spite of the stability, both bis(carbenes) are readily trapped by molecular oxygen to afford bis(ketones). Presumably, the reaction of the upper-lying localized quintet states with oxygen is much faster than that for lower-lying states. 相似文献
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The glucose receptor 1 developed by Shinkai was synthesized by known methods and with modifications involving the final synthetic step, installation of the phenylboronic acid moieties. Binding of the bis(alpha-hydroxycarbolxylate), tartrate, was assessed and compared to the corresponding bis(diol), erythritol, as well as the corresponding mono(alpha-hydoxycarboxylate), malate. These results suggest that bisboronate/bis(alpha-hydoxycarboxylate) interactions are stronger than the corresponding bisboronate/bis(diol) interactions. Furthermore, we report that the receptor is an order of magnitude more selective for tartrate than malate. 相似文献
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O. V. Andreev M. N. Bochkarev T. V. Nekrasova A. V. Protchenko 《Russian Chemical Bulletin》1995,44(2):233-235
X-ray amorphous samarium(II) sulfide was prepared by the reaction of H2S with samarium(II) bis[bis(trimethylsilyl)amide] (1) in THF at 10–2 Torr. Compound1 was prepared by two methods: 1) the reaction of SmI2 with lithium bis(trimethylsilyl)amide and 2) the reaction of samarium naphthalide with bis(trimethylsilyl)amine. SmS was transformed to the polycrystalline state with the lattice parametera = 5.92 Å by annealing at 400–500 °C.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 241–243, February, 1995. 相似文献
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Copper(II) and nickel(II) complexes of glyoxaldehyde bis{N(3)-methyl-, bis{N(3)-ethyl-, bis{N(3)-dimethyl-, bis{piperidyl-
and bis{hexamethyleneiminylthiosemicarbazone} have been prepared and studied spectroscopically. The five bis(thiosemicarbazones)
have been characterized by their melting points, as well as i.r., electronic and 1H-n.m.r. spectra. The four-coordinate copper(II)
complexes have been studied by e.s.r. spectroscopy, and the copper(II) and nickel(II) complexes by a number of the spectroscopic
techniques mentioned above. Upon formation of these complexes, loss of protons from each thiosemicarbazone moiety occurs,
and the bis(thiosemicarbazones) coordinate to the metal centres as dianionic, tetradentate N2S2 ligands.
This revised version was published online in June 2006 with corrections to the Cover Date. 相似文献