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十二烷基磺酸铁催化合成丙酸正丁酯 总被引:3,自引:1,他引:3
以十二烷基磺酸铁催化合成了丙酸正丁酯。实验结果表明最佳反应条件为:丙酸100mmol,n(丙酸):n(正丁醇)=1.0:1.2,十二烷基磺酸铁0.8g(约1.0mmol),带水剂环己烷6mL,回流分水60min,酯化率94.6%。催化剂重复使用5次仍保持较高活性。 相似文献
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用环境友好催化剂俣成丙酸苄酯的研究 总被引:16,自引:0,他引:16
应用环境友好催化剂H-β沸石催化苯甲醇与丙酸的酯化反应,合成了丙酯苄酯。研究结果表明,H-β沸石 具有较高的催化活性。考察了苯甲醇/丙酸摩尔比、催化剂用量、反应温度、反应时间和带水剂环己烷用量对酯产率的影响。在典型反应条件(苯甲醇/丙酸摩尔比=1.15:1、10.5gH-β沸石/摩尔丙酸、反应温度160℃ 、反应时间3.5h和20mL环己烷/摩尔丙酸)下,所得丙酸苄酯的产率为77%,该催化剂易于回收且可重复使用,具有良好的活性稳定性,并研究了用某些金属阳离子改性的β沸石的催化活性。 相似文献
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以乙酸乙酯为原料,在金属铑催化下与一氧化碳进行羰基化反应,生成丙酸。研究了碘化物添加剂和反应条件对丙酸产率的影响。由于避免了乙醇在酸性条件下的酯化和分子间脱水等副反应,丙酸产率显著提高。乙酸乙酯羰基化具有与甲醇羰基化相似的动力学行为。碘化物添加剂的加入能有效提高反应速率和丙酸选择性。通过优化反应条件,丙酸产率大于95%。 相似文献
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β—三氯锡基丙酸酯配合物和乙醇的酯交换反应研究田来进,田君廉,傅芳信(山东曲阜师大化学系曲阜273165)(东北师大化学系130024)关键词:β-三氯锡基丙酸酯,配合物,酯交换反应β-三氯锡基丙酸酯是一类新型的聚氯乙烯热稳定剂中间体,其配合物可望具... 相似文献
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硫酸高铈催化合成丙酸苄酯 总被引:8,自引:0,他引:8
以结晶硫酸高铈为催化剂对丙酸苄酯的合成进行了研究,考察了反应时间、催化剂用量、醇酸摩尔比和带水剂等因素对反应的影响,结果表明,在最佳反应条件下,酯化率在85%以上。 相似文献
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Ni-Zn/C催化剂上乙醇气相羰基化 总被引:9,自引:0,他引:9
对镍催化剂上常压下乙醇气相羰基化合丙酸及丙酸乙酯进行了研究,结果发现,Ni-Zn/C催化剂比Ni/C具有更高的活性与选择性,实验对催化剂中Ni及Zn含量进行了优化,Ni含量5%,Zn含量3.5%时最佳,考察了反应温度对产物分布的影响,结果表明250℃为最佳反应温度,采用程序升温脱附技术(TPD)对促进剂碘乙烷在活性炭,Ni/C,Zn/C及Ni-Zn/C上的行为进行了考察。实验结果表明,乙醇的甲烷化 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
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
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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
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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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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions. 相似文献
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献