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以1-甲基-3-乙基(-4-氯)-5-吡唑甲酰肼作原料,经两步得到4-氨基-3-(1-甲基-3-乙基(-4-氯)-5-吡唑基)-1,2,4-三唑-5-硫酮(3),3再与取代羧酸反应,得到一系列3-(1-甲基-3-乙基(-4-氯)-5-吡唑基)-6-取代均三唑并[3,4-b]-1,3,4-噻二唑(4、5、6).元素分析、1HNMR、IR和MS确定了它们的结构.初步生测结果表明:3具有植物生长调节活性,4b、4d、6具有杀菌活性. 相似文献
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Synthesis of 3,6-Disubstituted 5,6-Dihydro-s-triazolo [3,4-b]-1,3,4-thiadiazolidines through the Intramolecular Mannich Reaction 总被引:2,自引:0,他引:2
3-取代基-4-氨基-5-巯基-1,2,4-三唑在微量酸催化下与取代芳香醛经分子内Mannich反应合成了29个新的3,6-二取代-5,6-二氢-s-三唑并[3,4-b]-1,3,4-噻二唑啉类化合物,其结构经元素分析、IR和1HNMR进行确证,并讨论了反应的立体选择性。 相似文献
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2-(3,5-二氯-2-吡啶偶氮)-5-二甲氨基苯胺与铂(Ⅳ)显色反应的研究 总被引:8,自引:0,他引:8
研究了2-(3,5-二氯-2-吡啶偶氮)-5-二甲氨基苯胺(3,5-diCl-PADMA)与铂(Ⅳ)的显色反应及铂配合物的质子化行为。结果表明,在0.04~0.48mol/L的H2SO4溶液中,于加热的条件下,试剂可与铂(Ⅳ)形成稳定的1∶2绿蓝色PtL2H2+2配合物,其最大吸收波长位于634nm,表观摩尔吸光系数为9.73×104L·mol-1·cm-1,桑德尔灵敏度为0.002μg·cm-2。铂配合物的三级质子化常数分别为:lgKa1=3.91,lgKa2=-2.21,lgKa3=-3.37。较大量的常见金属离子及除钯、钌外的其它贵金属离子不干扰测定。利用Pt,Pd与试剂反应所需的温度差异,可以用差减法消除微量Pd的干扰.铂(Ⅳ)浓度在每10mL0~7.5μg范围内符合比尔定律。所拟方法用于二次合金管理样-88及催化剂中微量铂的测定,结果满意。 相似文献
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以2-羟基蒎烷-3-酮(1)与氨基乙腈缩合得到的手性酮亚胺(2)为中间体,经去质子化,在Pd(0)催化下与1,4-二氯-2-丁烯(3)发生串联反应,得到光学活性环丙烷衍生物(4),产率约为70%,反应的非对映立体选择性(d.e.)为100%.化合物4经选择性还原后水解,即可制得光学活性2-乙基环丙烷氨基酸,产物的对映体过量(e.e.)为33%. 相似文献
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包公藤甲素全合成的研究(Ⅱ)——中间体8-甲基-2β-羟基-8-氮二环[3.2.1]辛烷-6-exo-腈的合成 总被引:1,自引:1,他引:1
研究了N-甲基-3-羟基吡啶盐与丙烯腈的1,3-偶极环加成反应.由环合产物经过氢化,还原得包公藤甲素的中间体8-甲基-2β-羟基-8-氮二环[3.2.1]辛烷-6-exo-腈.本合成路线具有高立体选择性. 相似文献
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二代螺环树形化合物1,2,3,4,5,6,7,8,9,10,11,12-十二氢-2,2;6,6;10,10-三[3,3-二(烷氧羰基)-1,1-环亚丁基二甲氧基]三亚苯基的合成 总被引:1,自引:0,他引:1
以1,4-环己二酮、丙二酸二乙酯及多元醇等为原料, 经过两次“一锅煮”法合成了六种二代螺环树形化合物1,2,3,4,5,6,7,8,9,10,11,12-十二氢-2,2;6,6;10,10-三[3,3-二(烷氧羰基)-1,1-环亚丁基二甲氧基]三亚苯基螺环树形化合物, 其中烷氧基为异戊氧基、三羟甲基甲氧基、2,2-二溴甲基-3-羟丙氧基、2,2-二羟甲基丙氧基、二羟甲基膦甲氧基和(N-羟甲基-N-二羟甲基氨基乙基)甲氧基. 利用IR, NMR, MS和元素分析对合成的化合物进行了结构认证, 对影响反应的因素进行了讨论. 相似文献
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Jarmo Ropponen Tero Tuuttila Manu Lahtinen Sami Nummelin Kari Rissanen 《Journal of polymer science. Part A, Polymer chemistry》2004,42(22):5574-5586
The syntheses and thermal and X‐ray powder diffraction analyses of three sets of aliphatic polyester dendrimers based on 2,2‐bis(hydroxymethyl)propionic acid as a repeating unit and 2,2‐dimethyl‐1,3‐propanediol, 1,5‐pentanediol, and 1,1,1‐tris(hydroxymethyl)ethane as core molecules are reported. These dendritic polyesters were prepared in high yields with the divergent method. The thermal properties of these biodendrimers were evaluated with thermogravimetric analysis and differential scanning calorimetry. The thermal decomposition of the compounds occurred around 250 °C for the hydroxyl‐ended dendrimers and around 150 °C for the acetonide‐protected dendrimers. In addition, the crystallinity of the lower generation dendrimers was evaluated with X‐ray powder diffraction. The highest crystallinity and the highest melting points were observed for the first‐generation dendritic compounds. The higher generation dendrimers showed weaker melting transitions during the first heating scan. Only the glass‐transition temperatures were observed in subsequent heating scans. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 5574–5586, 2004 相似文献
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《Tetrahedron: Asymmetry》1999,10(10):1961-1968
The first enantioselective double nucleophilic addition reaction to O-protected cyanohydrin was achieved in 71% yield and 82:18 enantiomeric ratio by using a bis(BINOL)titanium Lewis acid complex. New (4S,5S)-2,2-dialkyl-4,5-bis(hydroxymethyl)-1,3-dioxolane titanium complexes were synthesized and they displayed good levels of enantioselection in the nucleophilic addition reaction. 相似文献
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Ferguson A Schmidtmann M Brechin EK Murrie M 《Dalton transactions (Cambridge, England : 2003)》2011,40(2):334-336
We describe the first use of Bis-tris propane {2,2'-(propane-1,3-diyldiimino)bis[2-(hydroxymethyl)propane-1,3-diol], H(6)L}, in nickel and cobalt chemistry and report the synthesis, structure and magnetic properties of [Ni(4)(H(4)L)(H(3)L)(acac)(2)](+) (1) and [Co(II)(3)Co(III)(2)(H(2)L)(2)(acac)(3)(MeOH)](+) (2). 相似文献
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Bis(azafulvene) was isolated in 55% yield by the reaction of 4 equivalents of phenyllithium with 5,5'-diformyl-3,3',4,4'-tetraethyl-2,2'-bipyrrole followed by quenching with acetic anhydride. Unstable bis(azafulvene)s were obtained in much higher yields by dehydrating 5,5'-bis(hydroxymethyl) derivatives of 2,2'-bipyrrole and gem-dimethyl-2,2'-dipyrrylmethane with (Boc)2O-DMAP at room temperature. X-Ray crystallography of two bis(azafulvene)s is reported. 相似文献
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Habib Firouzabadi Nasser Iranpoor Hassan Hazarkhani 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):2847-2858
A new application of solid silica chloride, an easily available and efficient catalyst for the preparation of diacetal of 2,2-bis-(hydroxymethyl)-1,3-propanediol from aldehydes, acetals, acylals, and oximes, is described. Transthioacetalization of diacetals of 2,2-bis-(hydroxymethyl)-1,3-propanediol into their corresponding 1,3-dithianes and 1,3-dithiolanes in the presence of silica chloride is presented. Efficient regeneration of carbonyl compounds from their corresponding acetals, ketals, diacetals, and acylals in the presence of this catalyst also is described. 相似文献
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I. V. Shchur O. G. Khudina Ya. V. Burgart V. I. Saloutin M. A. Grishina V. A. Potemkin 《Russian Journal of Organic Chemistry》2007,43(12):1781-1787
New fluoroalkyl-containing 2,2′-(biphenyl-4,4′-diyldihydrazono)bis(1,3-diketones) and 2,2′-(biphenyl-4,4′-diyldihydrazono)bis(3-oxopropionates) were synthesized by azo coupling of the corresponding 1,3-dicarbonyl compounds with biphenyl-4,4′-bis(diazonium) dichloride. Complexing ability of the obtained bis-hydrazones was studied, and new coordination compounds of the general formula M2L2 [where M = Ni(II), Cu(II); L = fluoroalkyl-containing 2,2′-(biphenyl-4,4′-diyldihydrazono)bis(1,3-diketone)] were obtained. 相似文献