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1.
以廉价的2-溴苯甲醚制取了格氏试剂,通过Kumada偶联反应得到2-噻吩基苯甲醚,再通过吡啶盐酸盐脱甲基得到2-噻吩基苯酚。从催化剂、配体、溶剂等方面对Kumada偶联反应进行了筛选和优化,结果表明Kumada偶联反应时,72℃以Pd(dppf)Cl2(0.001 mol)为催化剂(dppf,二茂铁),三苯基膦(PPh3)和1,1’-双(二苯基膦)二茂铁(dppf)作为配体,四氢呋喃和乙二醇二甲醚为混合溶剂,反应16 h,得到2-噻吩基苯甲醚,纯度95%,产率65%。再通过吡啶盐酸盐脱甲基得到2-噻吩基苯酚,纯度大于98%,产率65%。该方法原料便宜,后处理简单,收率较高。 相似文献
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N,N-二甲基-1,3-丙二胺与单氰胺经亲核加成反应制得中间体N,N-二甲基-N′-胍基-1,3-丙二胺(2); 以壳聚糖为起始原料,依次与氯乙酸、环氧氯丙烷经取代反应制得N-(1-羟基-3-氯丙基)-羧甲基壳聚糖(4); 4与2经季铵化反应合成了一系列含有胍基和季胺基团的羧甲基壳聚糖衍生物(5),其结构经1H NMR, IR和元素分析表征。研究了反应配比[γ=m(2)∶m(4)]和反应时间对5取代度的影响,结果表明,当γ为3∶1,反应时间为10 h时,取代度最高(73%)。 相似文献
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合成了两个新型的艾溴利平类似物——N-2 -硝基-4-氯苯基-4-[(膦酸二乙酯基)甲基]苯甲酰肼(5,总收率28.1%)和N-2-四氮唑基-4-氯苯基-4-[(膦酸二乙酯基)甲基]苯甲酰胺(7,总收率30.5%).以对氯甲基苯甲酸为原料,经酯化、水解和酰氯反应制得中间体4-[(膦酸二乙酯基)甲基]苯甲酰氯(4);4与2-硝基-4-氯苯肼盐酸盐反应合成了5.4先与2-氨基-5-氯苯腈反应制得N-2-氰基-4-氯苯基-4-[(膦酸二乙酯基)甲基]苯甲酰胺(6);6再与叠氮化钠反应合成了7.其结构经1 H NMR和IR表征. 相似文献
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将壳聚糖改性为(2-羟基-3-丁氧基)丙基 羟丙基壳聚糖(2-H-3-B-P-HPCS),并以(2-羟基-3-丁氧基)丙基-羟丙基壳聚糖和聚乙二醇(PEG)为原料制备(2-羟基-3-丁氧基)丙基-羟丙基壳聚糖/聚乙二醇互穿网络凝胶,研究了(2-羟基-3-丁氧基)丙基-羟丙基壳聚糖浓度、聚乙二醇的用量、交联剂戊二醛用量、反应温度对该凝胶溶胀性能的影响。 通过红外光谱分析和扫描电子显微镜的方法比较了壳聚糖、(2-羟基-3-丁氧基)丙基-羟丙基壳聚糖和(2-羟基-3-丁氧基)丙基-羟丙基壳聚糖/聚乙二醇互穿网络凝胶结构和形态上的不同。 以阿昔洛韦为模型药物研究了其释药性能。 结果表明,该凝胶均具有良好的溶胀性、pH敏感性和药物缓释作用,有望用作新型的药物载体。 相似文献
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本文研究了在Pd(PPh3)2Cl2(1)催化下的三正丁基-2-呋喃基锡(6a), 三正丁基-2-噻吩基锡(6a), 三正丁基-2-(N-甲基)吡咯基锡(6c)和菊酰氯(5), 肉桂酰氯(7)的交联反应。发现除了三正丁基-2-(N-甲基)吡咯与5的不寻常反应得到2, 5-二取代的吡咯衍生物外, 其余反应皆以70~87%的产率得到交叉偶联产物。本文同时还报道了钯催化下有机锡试剂与取代卤代芳烃反应, 高收率地得到了不对称的杂环基芳烃和双杂环化合物。在合成的交联产物中, 化合物2, 8, 9, 15, 16与17均为新化合物。 相似文献
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以罗丹明B为原料,通过两步法合成化合物N-(3’,6’-双(二乙基氨基)-3-氧杂螺环[异二氢吲哚-1,9’-氧杂蒽]-2-酰基)-4-甲氧基苯甲酰胺(RHL)。通过罗丹明B酰肼(RA)与对甲氧基苯甲酰氯反应的单因素考察,得到最优合成条件:反应溶剂为乙酸乙酯,反应温度80℃,三乙胺作为缚酸剂,反应时间10 h,投料比n(RA)∶n(对甲氧基苯甲酰氯)=1.0∶1.3。通过测定溶剂、 pH、金属离子对化合物RHL荧光强度的影响,发现RHL在乙醇-水(1∶1, V/V)体系中,pH在1.50~7.02范围内发射出新的强烈的橙红色荧光,RHL对pH的荧光传感具有良好的选择性和重复性,且绝大多数金属离子对体系无干扰。 相似文献
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改性壳聚糖树脂对利尿剂的吸附性能 总被引:5,自引:0,他引:5
用琥珀酸酐、苯甲酸酐、聚乙烯亚胺和 3 氯 2 羟丙基三甲基氯化铵对壳聚糖进行改性 ,分别在其氨基上引入羧基、苯环、多氨基和季胺基 ,并利用红外谱图对于改性后的壳聚糖的结构进行了分析 .应用相转移法制备了 4种改性壳聚糖的微球 ,实验研究了这 4种微球对 9种不同利尿剂的吸附性能 .结果表明 ,由于Lewis酸碱相互作用 ,引入羧基后的壳聚糖树脂对 3种碱性利尿剂的吸附量有了 15 %~ 36 %的提高 ,而引入多氨基的壳聚糖树脂对四种酸性利尿剂的吸附量分别提高了 4 8 5 %~ 2 0 9% ;由于苯环和利尿剂的憎水性基团的相互作用 ,引入苯环后的壳聚糖树脂对所有的利尿剂的吸附量都有所提高 ,其幅度为 15 %~ 6 1% ;因为季胺基团和羧基之间发生的离子交换作用 ,引入季胺基后的树脂对具有羧基的利尿剂吸附量有显著的提高 ,尤其对布美它尼的吸附量提高了 2倍以上 . 相似文献
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生物降解多功能缓释微球的制备与表征 总被引:6,自引:1,他引:5
通过羧甲基壳聚糖接枝二甲基十八烷基环氧丙基氯化铵, 合成水油两溶性的羧甲基壳聚糖十八烷基季铵盐(OQCMC); 并将其作为乳化剂与乳酸-羟基乙酸(PLGA)和羟乙基纤维素(HEC)复合, 利用溶剂挥发法, 构建一种多功能的药物载体缓释系统, 并尝试包裹脂溶性药物盐酸米诺环素. 利用Transmission electron microscopy, Quasielastic laser light scattering, Zeta电位仪, FTIR, 1H NMR等对OQCMC及载药微球进行表征, 并进行药物的体外释放实验. 结果表明: OQCMC可作为一种优良的乳化剂对PLGA微球进行修饰; 并可使复合微球体系带正电, 在提高微球载药率(9.4%)的同时减小微球粒径[(166.4±0.8) nm]; 复合微球体系对盐酸米诺环素具有较好的物理包裹能力, 并有长效缓释作用(PBS, pH=7.9). 相似文献
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Two oxime-cyclophosphazenes were prepared from hexakis(4-formylphenoxy)cyclotriphosphazene (2) and hexakis(4-acetylphenoxy)cyclotriphosphazene (7). The reactions of these oximes with benzyl chloride, benzenesulfanoyl chloride, benzoyl chloride, 4-methoxybenzoyl chloride and 2-chlorobenzoyl chloride were studied. Hexa and pentasubstituted compounds were obtained from the reaction of hexakis(4-[(hydroxyimino)methyl]phenoxy)cyclotriphosphazene (3) with benzyl chloride (4) and benzoyl chloride, respectively. However, the oxime groups on 3 rearranged to nitrile (5) in the reaction of 3 with benzenesulfanoyl chloride and 1-napthalenesulfanoyl chloride. Hexasubstituted compounds were also obtained from the reactions of hexakis(4-[(1)-N-hydroxyethaneimidoyl]phenoxy)cyclotriphosphazene (8) with benzoyl chloride (10), 4-methoxybenzoyl chloride (11) and 2-chlorobenzoyl chloride (12). A trisubstituted compound was obtained from the reaction of 8 with benzyl chloride (9). All the products were generally obtained in high yields. Pure and defined products could not be obtained from the reaction of 3 with 4-methoxybenzoyl chloride and 2-chlorobenzoyl chloride. The structures of the compounds were defined by elemental analysis, IR, 1H, 13C and 31P NMR spectroscopy. 相似文献
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Ahmed A. El‐Barbary Mahmoud A. El‐Badawi Yasser M. Loksha 《Journal of heterocyclic chemistry》2001,38(3):711-716
Some novel 3,7‐dimethyl‐6H‐pyrazolo[5,1‐c][1,2,4]triazin‐4‐ones were prepared (3a‐g) . Compounds 3a,b were treated with hydrazines to afford various products 7a,b, 8a,b, 9 and lla,b depending on the type of hydrazine derivative and reaction conditions. The benzoyloxyimino‐pyrazolo[5,1‐c][1,2,4]triazines (13a,b) were synthesized by refluxing of compounds 3a,b with hydroxylamine hydrochloride to afford the corresponding oxime derivatives followed by treatment with benzoyl chloride. 相似文献
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Seven new anionic triphenytin complexes, triethylammonium (organocyanoamino)chlorotriphenylsannates, were prepared by the reaction of (triphenylstannyl) cyanamide with acid chlorides, alkyl chlorocarbonates, or benzenesulfonyl chloride in the presence of triethylamine. One of these complexes, triethylammonium (acethylcyanoamino)chlorotriphenylstannate, was also prepared by the reaction of triethylamine hydrochloride with N-(triphenylstannyl)-N-acetylcyanamide, which was obtained by following acetyl chloride to react with bis(triphenylstannyl)carbodiimide. The PMR and IR (4000-140 cm?1) spectrum of each complex was measured. The Mössbauer parameters of two of the complexes were obtained, the quadrupole splittings being consistent with trigonal bipyramidal structures. p-Nitrobenzoyl chloride and terephthalyl chloride failed to give complexes on reaction with (triphenylstannyl)cyanamide and triethylamine, but instead gave the triethylammonium salt of the corresponding acylcyanamide. The new anionic complex, triethylammonium dichlorotriphenylstannate, was prepared by the reaction of triphenyltin chloride with triethylamine hydrochloride. 相似文献
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《印度化学会志》2021,98(9):100129
The modification of chitosan in ionic liquids through homogeneous reactions has advantages including shorter time and simple post-treatment and the generated chitosan derivatives have high degrees of subsititution and good reproducibility. In this paper, we studied the reaction kinetics of glycidyl trimethyl ammonium chloride and chitosan in 1-allyl-3-methylimidazolium chloride. Chitosan concentration, temperature, and reaction time were studied to determine their influence on reaction kinetics. The results indicated that reaction rate increased with increases of both chitosan concentration and temperature. A first-order kinetics equation was generated, where the relationship between reaction rate constant and temperature was determined. 相似文献
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Yu. S. Tsizin N. L. Sergovskaya S. A. Chernyak 《Chemistry of Heterocyclic Compounds》1986,22(4):421-424
1-Alkyl(aralkyl)-4-acyl-2-piperazinones are formed in high yields during selective acylation of N-monosubstituted ethylenediamines by benzoyl and cyclohexylcarbonyl chlorides in the presence of pyridine hydrochloride and treatment of the reaction products with chloroacetyl chloride in the presence of potassium tert-butylate.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 514–517, April, 1986. 相似文献
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Cai Qin QIN Ling XIAO Yu Min DU* Department of Environmental Science Wuhan University Wuhan 《中国化学快报》2001,(12)
Borohydride exchange resin (BER) a useful reducing reagent has been used in reduction of some carbonyl compounds and acyl halides1. When BER combines with a transition metal catalyst, it can reduce C=C double bonds2, halides2, nitro compounds3, cyano, diazo3 and azide compounds4. The support of BER is the synthetic macromolecule polystyrene. Here, we used chitosan as the support of borohydride. As known, chitosan is a renewable and abundant natural polysaccharide. Scheme 1 Preparat… 相似文献
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Chloroacylation and bromoacylation of carbonyl compounds IV. Investigations of the reaction mechanism The kinetics of the Lewis acid catalyzed reaction between acyl chlorides and carbonyl compounds (especially aldehydes) is investigated by 1H-NMR.-spectroscopy. With acetyl chloride as starting material a second order reaction is observed; the rate of the reaction increases in polar solvents as well as with increasing electron-donating capacity of the aldehyde. - With benzoyl chloride as starting material the reaction is first order with respect to benzoyl chloride, but zero order with respect to the aldehyde. The reaction rate is strongly influenced by the substituents of the benzoyl chloride. - Two polar reaction mechanisms which are in accord with these results are outlined and discussed. 相似文献