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1.
对硝基苯磺酰基乙腈与芳香醛在3-N,N-二甲基-1,3-丙二胺(DPA)/冰醋酸催化下可顺利地发生Knoevenagel缩合反应,生成2-(4-硝基苯磺酰基肉桂腈类化合物,产率83%~98%。但与水杨醛反应生成的产物是六元环内酯,其结构经元素分析、IR、 ̄1HNMR和MS确证。  相似文献   

2.
在K2CO3-TEBA-DMF体系中,2-(2-氯-4-硝基苯磺酰基)-1-芳基乙酮与各种灶基化试剂发生烷基化-环化反应,得到一系列3-位取代的1,4-氧硫要萘-4,4-二氧化物,并讨论了反应机理和反应条件。  相似文献   

3.
通过3-苄基-4-芳酰基-1,2,4-三唑-5-巯基负离子在2-甲磺酰基-5-苯基-1,3,4-E二唑环2-位上的亲核取代反应,制得13个新的(3-苄基-4-芳酰基-1,2,4-三唑-5-基)(5-苯基-1,3,4-E二唑-2-基)硫醚衍生物。经元素分析、IR、^1H NMR和MS裂解碎片分析确认结构。初步观察了它们在0.01%浓度时对大肠杆菌繁殖的抑制作用。  相似文献   

4.
在固液相转移催化(K2CO3/DMF/TEBA)条件下,对硝基苯磺酰基乙酸酯与α、β-不饱和酸酯反应意外地生成加成重排产物。其反应机理可能是砜酯首先与α、β-不饱和酯起Michael反应,随后加成物发生分子内芳环上的新核性取代,酸化后脱去SO2得最终产物。  相似文献   

5.
胡Min  刘勇 《合成化学》1998,6(2):150-154
介绍了带羟基桥连双-(中环多胺)的合成,首先利用N-对甲苯磺酰基-3-羟基-1,5-二杂环庚烷与5种双官能基化合物在N2气氛下无水乙腈中反应,得到5种带对甲苯磺酰基的中环多胺,然后利用HBr/HOAc脱去保护基团,得到桥连双-(中环多胺)的氢溴酸盐,所有新化合物的结构均经IR,^1HNMR,MS或元素分析证实。  相似文献   

6.
李小华  胡宏纹 《合成化学》1996,4(2):161-163
由N-苯磺酰基甲基苯胺与芳醛反应得到了7种缩合产物,其结构经元素分析,HNMR,MS和IR所确证。  相似文献   

7.
在固液相转移催化(K_2CO_3/DMF/TEBA)条件下,对硝基苯磺酰基乙酸酯与α,β-不饱和酸酯反应意外地生成加成重排产物[如生成2-甲基-2-(对硝基苯基)戊二酸-1-甲酯-5-乙酯]。其反应机理可能是砜酯首先与α,β-不饱和酯起Michael反应,随后加成物发生分子内芳环上的亲核性取代,酸化后脱去SO2得最终产物。  相似文献   

8.
研究了新型感光稳定剂N,N’-二(芳磺酰)亚磺酰胺-S-(2-苯并咪唑)钠(芳磺酰基为苯磺酰,对甲苯磺酰,对氯苯磺酰)与增感染料在实用照相乳剂虽的超增感与防雾作用。  相似文献   

9.
通过1-苯基本磺酰基硫脲(1)与亚磷酸三苯酯和取代苯甲醛在甲苯中进行的类Mannich反应合成1-对甲苯磺酰基-2-氧代-2-苯氧基-3-芳基-1,4,2-二氮磷杂环戊-5-硫酮(2)。本文对合成过程中所涉及到的副反应进行了初步探讨。  相似文献   

10.
芳胺常压气相N—烷基化反应研究   总被引:1,自引:0,他引:1  
在固定床催化反应器中常压下研究了芳胺和醇的气相法N-烷基化反应。考察了γ-Al2O3系列催化剂的反应性能,筛选出了两种适用于苯胺N-甲基化反应且性能较好的催化剂。反应条件为:在甲醇和苯胺的摩尔比为3:1时,反应温度为280℃,液时空速为0.3h^-1的条件下,苯胺转化率为99%,生成N,N-二甲基苯胺(DMA)的选择性为92%。研究了甲醇和芳环上不同位置取代的甲基苯胺的反应规律,其转化率顺序:苯胺  相似文献   

11.
用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.  相似文献   

12.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

13.
A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.  相似文献   

14.
A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.  相似文献   

15.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

16.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

17.
The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.  相似文献   

18.
Siqi Li  Xingpeng Chen  Jiaxi Xu 《Tetrahedron》2018,74(14):1613-1620
Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular SN2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively.  相似文献   

19.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

20.
N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).  相似文献   

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