Electrocatalytic synthesis of gem-bisarylthio enamines and α-phenylthio ketones via a radical process under mild conditions

Synlett ◽  
2020 ◽  
Author(s):  
Yong-Zhou Pan ◽  
Shi-Yan Cheng ◽  
Qian-Yu Li ◽  
Hai-Tao Tang ◽  
Ying-Ming Pan ◽  
...  

The novel method for the synthesis of gem-bisarylthio enamines and α-phenylthio ketones was developed via the coupling of α-substituted vinyl azides with thiols in the presence of tetrabutylammonium iodide (TBAI) as a redox catalyst and electrolyte at room temperature. Electronic properties were crucial in the generated products. This protocol features metal- and oxidant-free materials, broad tolerance of substrates, and mild reaction conditions.

2011 ◽  
Vol 396-398 ◽  
pp. 1283-1286
Author(s):  
Jian Peng Zhu ◽  
Chun Hu Li ◽  
Jia Ling Chen ◽  
Ying Wei Luo

Abstract. Investigation of polymer resin as catalyst in the oxidative desulfurization (ODS) process has revealed that the method can be applied to make a relative high removal of sulfur compounds. The reaction conditions, including temperature, amount of oxidant and reaction time were studied. The best result occurs under mild conditions with respect to room temperature and atmospheric pressure, to remove 75.54% of the totle sulfur content in the presence of H2O2 with an O/S molar ratio of 17. Possible mechanism is also disscussed.


2021 ◽  
Author(s):  
Jianguo liu ◽  
Shanshan Lin ◽  
Longlong Ma

Aniline is a group of important platform molecules and is widely used in the synthesis of other high-value chemicals and pharmaceutical products. How to produce high-value anilines as the high-value chemical intermediates more efficiently and more environmentally has always been a research topic in the industry. Catalytic hydrogenation is an environmentally friendly method for preparing halogenated anilines. Traditional noble metals catalysis face cost and noble metals residue problems. To improve the purity of the product and the activity and recyclability of the catalyst, we prepared a Pd/Fe magnetic bimetallic catalyst supported on N-doped carbon materials to reduce nitrobenzene to aniline under mild conditions. The loading of Pd was very low, which was 1/10 of the content of common commercial precious metal Pd/C and Pt/C catalysts, which was only 0.5%. And the prepared bimetallic Pd/Fe@N/C catalyst showed excellent catalytic reactivity with the conversion rate of nitrobenzene > 99%, and the selectivity of aniline 99% under mild reaction conditions of 0.8 MPa H2 and 40 °C. A variety of halogenated and aliphatic nitro compounds were well tolerated and had been transformed to the corresponding target amine products with excellent selectivity. In addition, the novel N-doped graphene-encapsulated bimetallic magnetic Pd/Fe@N/C catalyst not only had magnetic physical properties, which was easy to separate, recover, and used for the recycling of the catalyst without metal leaching but also catalyzed highly selective reductive amination of aromatics was a green, economical and environmentally friendly reaction with the only H2O as a by-product.


2007 ◽  
Vol 336-338 ◽  
pp. 165-168 ◽  
Author(s):  
Jeremie Barrel ◽  
Eugene Stytsenko

Ferroelectric thick films of Bi3NbTiO9 (BNT) with Aurivillius type structure were fabricated using the airflow deposition method at room temperature. The precursor powder for deposition was prepared by a conventional mixed oxide route. The BNT films obtained from airflow deposition had thickness between 25 and 90 μm. Subsequent sintering showed that the films were sinterable at lower temperatures than bulk samples prepared from the same powder using isostatic cold pressing technique. Thick films sintered at 900 0C displayed higher density and a higher electrical breakdown field compared with bulk samples. SEM microscopy showed similar grain size for the thick films sintered at 900 0C and corresponding bulk samples sintered at 1150 0C. A pronounced preferential grain orientation of 70% along the c-axis was observed for thick films with thickness of 252m sintered at 9000C. While the grain orientation in bulk samples was random the grains in the thick films were aligned along the substrate plane. This significant microstructural difference between thick film and bulk samples is believed to be associated with directional nature of the deposition process. The novel method allowed anisotropic film formation without applying pressure during sintering. Low sintering temperature allows reduction in bismuth losses and better grain growth control, which also contributes to the advantages of the method.


2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Diego M. Ruiz ◽  
Juan C. Autino ◽  
Nancy Quaranta ◽  
Patricia G. Vázquez ◽  
Gustavo P. Romanelli

We report a suitable quinoxaline synthesis using molybdophosphovanadates supported on commercial alumina cylinders as catalysts. These catalysts were prepared by incipient wetness impregnation. The catalytic test was performed under different reaction conditions in order to know the performance of the synthesized catalysts. The method shows high yields of quinoxaline derivatives under heterogeneous conditions. Quinoxaline formation was obtained using benzyl,o-phenylenediamine, and toluene as reaction solvent at room temperature. The CuH2PMo11VO40supported on alumina showed higher activity in the tested reaction. Finally, various quinoxalines were prepared under mild conditions and with excellent yields.


2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Jiufang Duan ◽  
Chunrui Han ◽  
Liujun Liu ◽  
Jianxin Jiang ◽  
Jianzhang Li ◽  
...  

A novel cellulose-chitosan gel was successfully prepared in three steps: (1) ferrocene- (Fc-) cellulose with degrees of substitution (DS) of 0.5 wt% was synthesised by ferrocenecarboxylic acid and cellulose within dimethylacetamide/lithium chloride (DMAc/LiCl); (2) theβ-cyclodextrin (β-CD) groups were introduced onto the chitosan chains by reacting chitosan with epichlorohydrin in dimethyl sulphoxide and a DS of 0.35 wt%; (3) thus, the cellulose-chitosan gel was obtained via an intermolecular inclusion interaction of Fc-cellulose andβ-CD-chitosan in DMA/LiCl, that is, by an intermolecular inclusion interaction, between the Fc groups of cellulose and theβ-CD groups on the chitosan backbone at room temperature. The successful synthesis of Fc-cellulose andβ-CD-chitosan was characterised by13C-NMR spectroscopy. The gel based onβ-CD-chitosan and Fc-cellulose was formed under mild conditions which can engender autonomous healing between cut surfaces after 24 hours: the gel cannot self-heal while the cut surfaces were coated with a solution of a competitive guest (adamantane acid). The cellulose-chitosan complex made by this method underwent self-healing. Therefore, this study provided a novel method of expanding the application of chitosan by binding it with another polymer.


2008 ◽  
Vol 86 (5) ◽  
pp. 376-383 ◽  
Author(s):  
Hamid Reza Shaterian ◽  
Asghar Hosseinian ◽  
Majid Ghashang

A one-pot, three-component condensation of an aryl aldehyde, an enolizable ketone or β-keto ester, acetyl chloride, and acetonitrile or benzonitrile in the presence of magnesium hydrogensulfate as an active, recoverable, and reusable green catalyst is described for the synthesis of β-amido ketones/esters at room temperature. The key features of this methodology are simplicity, mild reaction conditions, and high to excellent yields.Key words: multi-component reaction, magnesium hydrogensulfate, heterogeneous catalyst, β-amido ketone/ester, mild conditions.


2005 ◽  
Vol 58 (8) ◽  
pp. 611 ◽  
Author(s):  
Jun Wang ◽  
Xiao-Peng Miao ◽  
Gu Yuan

Propargylation of carbonyl compounds to produce homopropargylic alcohols plays a very important role in synthetic organic and pharmaceutical chemistry. A novel method that carbonyl compounds and propargyl halide were mediated by SnCl2/NiCl2-KI in water at room temperature was developed by us to successfully synthesize homopropargylic alcohols in good yields. The reactions were carried out in an environmentally friendly solution and under mild conditions.


Synthesis ◽  
2019 ◽  
Vol 51 (10) ◽  
pp. 2171-2182 ◽  
Author(s):  
Surabhi Gupta ◽  
Siddharth Baranwal ◽  
Nalluchamy Muniyappan ◽  
Shahulhameed Sabiah ◽  
Jeyakumar Kandasamy

N-Arylation of sulfoximines with different arylboronic acids, including sterically hindered boronic acids, is achieved using copper(I) iodide and 4-DMAP at room temperature. Moreover, N-arylation of biologically relevant l-methionine sulfoximine is demonstrated for the first time. All these reactions provided the desired products in excellent yields within a short span of time. The optimized reaction conditions are well suited to the task of N-vinylation of sulfoximine with trans-2-phenylvinylboronic acid.


2011 ◽  
Vol 8 (s1) ◽  
pp. S495-S501 ◽  
Author(s):  
Seied Ali Pourmousavi ◽  
Majid Hadavankhani ◽  
Zahra Zinati

A rapid and efficient method for the transthioacetalization of acylals (1,1-diacetates) and acyclic and cyclic acetals is described. The reaction was carried out using 1-benzyl-4-aza-1-azoniabicyclo[2.2.2]octane tribromide (1 mol%). The yield of the transthioacetalization was high and reaction conditions involve the use of acetonitrile as the solvent at room temperature; isolation is simple and the products are nearly pure.


Synthesis ◽  
2018 ◽  
Vol 50 (15) ◽  
pp. 2999-3005 ◽  
Author(s):  
Wenjun Lu ◽  
Chong Mei ◽  
Yixin Hu

Imides are prepared conveniently by visible-light-driven oxidations of various N-alkylamides under mild conditions. The majority of the reactions proceed efficiently by using Oxone as the oxidant in the presence of a catalytic amount of KBr in H2O/CH2Cl2 under irradiation by an 8 W white LED at room temperature. Experimental studies suggest that an imine, obtained from the substrate amide via a radical process, is the key intermediate.


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