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1

Chen, Longrui. "Development of Solvent-free Catalyzed Organic Reaction under Mechanochemical Conditions." University of Cincinnati / OhioLINK, 2016. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1470044218.

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2

Mossaraf, Hossain. "Solvent free synthesis of some heterocycles and their applications." Thesis, University of North Bengal, 2017. http://ir.nbu.ac.in/handle/123456789/2621.

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3

Grätz, Sven, Doreen Beyer, Valeriya Tkachova, Sarah Hellmann, Reinhard Berger, Xinliang Feng, and Lars Borchardt. "The mechanochemical Scholl reaction – a solvent-free and versatile graphitization tool." Royal Society of Chemistry, 2018. https://tud.qucosa.de/id/qucosa%3A70655.

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Herein, we report on the mechanochemical Scholl reaction of dendritic oligophenylene precursors to produce benchmark nanographenes such as hexa-peri-hexabenzocoronene (HBC), triangular shaped C60 and expanded C222 under solvent-free conditions. The solvent-free approach overcomes the bottleneck of solubility limitation in this well-known and powerful reaction. The mechanochemical approach allows tracking the reaction process by in situ pressure measurements. The quality of produced nanographenes has been confirmed by MALDI-TOF mass spectrometry and UV-Vis absorption spectroscopy. This approach paves the way towards gram scale and environmentally benign synthesis of extended nanographenes and possibly graphene nanoribbons suitable for application in carbon based electronics or energy applications.
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4

Aono, Shinji. "Theoretical Study of Electrostatic Solvent Effects within Free Energy Expression and Application to Solvated Reaction." 京都大学 (Kyoto University), 2010. http://hdl.handle.net/2433/126827.

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5

Botti, Luca. "Mechanochemical solvent-free synthesis of Sn-β Zeolite and Ag2O/TiO2 catalysts." Master's thesis, Alma Mater Studiorum - Università di Bologna, 2016. http://amslaurea.unibo.it/11941/.

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Preparations of heterogeneous catalysts are usually complex processes that involve several procedures as precipitation, crystallization and hydrothermal treatments. This processes are really dependent by the operative conditions such as temperature, pH, concentration etc. Hence the resulting product is extremely affected by any possible variations in these parameters making this synthesis really fragile. With the aim to improve these operations has been decided to exploit a new possible strong environment-respectful process by mechanochemical treatment, which permits to carry out solvent free-solvent synthesis exploiting the Mixer Mill MM400 (Retsch) in order to have reproducible results. Two different systems have been studied in this kind of synthesis: a tin β -zeolite tested in a H-trasnfer reaction of cyclohexanone and a silver on titania catalyst used in the fluorination of 2,2 dimethyl glucaric acid. Each catalyst has been characterized by different techniques in order to understand the transformations involved in the mechanochemical treatment.
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6

Liu, Pengyuan. "Development of Ambient Mass Spectrometry for Protein/Peptide Characterization, Solvent-Free Analysis, and Electrochemical Reaction Monitoring." Ohio University / OhioLINK, 2015. http://rave.ohiolink.edu/etdc/view?acc_num=ohiou1419335862.

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7

Machover, Sarah B. "Understanding the Solvent-free Nucleophilic Substitution Reaction Performed in the High Speed Ball Mill (HSBM): Reactions of Secondary Alkyl Halides and Alkali Metal-Halogen Salts." University of Cincinnati / OhioLINK, 2011. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1307043848.

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8

Strompen, Simon [Verfasser], and Andreas [Akademischer Betreuer] Liese. "Process development of a solvent-free, chemoenzymatic reaction sequence for the enantioselective synthesis of beta-amino acid esters / Simon Strompen. Betreuer: Andreas Liese." Hamburg-Harburg : Universitätsbibliothek der Technischen Universität Hamburg-Harburg, 2012. http://d-nb.info/1048542920/34.

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9

Mukherjee, P. "Solvent-free, triphase catalytic oxidation reactions over TS-1/H2O2 system." Thesis(Ph.D.), CSIR-National Chemical Laboratory, Pune, 2000. http://dspace.ncl.res.in:8080/xmlui/handle/20.500.12252/2277.

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10

Hopgood, Heather M. "Substitution Reactions in the High Speed Ball Mill." University of Cincinnati / OhioLINK, 2016. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1479816113315302.

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11

Grilly, Joshua David. "Switchable Solvents for Novel Chemical Processing." Thesis, Georgia Institute of Technology, 2005. http://hdl.handle.net/1853/7461.

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This work seeks to develop new solvents for environmentally benign chemical synthesis. Switchable solvents are a new class of compounds that change properties upon the application of some stimulus such as heat, UV light, or pH. We have developed the use of a new solvent, thiirane oxide, that has chemical properties similar to DMSO. Thiirane oxide, however, undergoes facile decomposition to two gases at temperatures above 100 C, which is much lower than the temperature required for removing DMSO. Thus we have a solvent with excellent solvation properties, but with a built-in switch for easier removal. However, thiirane oxide leaves behind sulfurous products which make the reverse reaction to reform the solvent unfeasible. We are also developing the use of another solvent, piperylene sulfone, which is expected to have good solvent properties, yet with decomposition products that can be reacted to reform the solvent. This thesis also details the work to date on piperylene sulfone. Gas-expanded liquids (GXLs) also show promise as a new reaction medium. In order to design solvent systems that take full advantage of this medium, we desire to understand the microstructure of these fluids. To that end, we are using cage reactions to probe solute-solvent and solvent-solvent interactions at the molecular level. This thesis discusses the current research on using cage reactions to probe the structure of GXLs.
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12

Venturini, Chiara. "On-surface coupling reactions on calcium carbonate." Thesis, Toulouse 3, 2015. http://www.theses.fr/2015TOU30158/document.

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Le couplage covalent sur surface métallique en UHV (Ultra High Vacuum) est une technique émergente permettant de synthétiser des structures moléculaires impossibles à obtenir par la chimie en solution (nanorubans de graphène, polymères 2D par exemple). Aujourd'hui, le plus grand défi reste le développement de ces réactions sur des surfaces isolantes pour différentes applications comme, par exemple, l'électronique moléculaire. En particulier, le couplage de dérivés d'acides benzoïques, greffés sur les surfaces de carbonate de calcium en UHV par des groupes carboxyliques, a été démontré récemment pour la première fois. Lors de ces travaux, nous avons dans un premier temps synthétisé des molécules précurseurs de réactions de couplage (homo-couplage d'éthyne, photopolymérisation, polycondensation et réaction d'Ullmann) sur des surfaces de carbonate de calcium en UHV. Par la suite, nous avons mené cette étude à l'échelle macroscopique (semi-préparatoire), par greffage de molécules sur des microparticules de carbonate de calcium, puis activation de la réaction, et enfin dissolution du substrat afin d'extraire le produit final. Les microparticules ont été obtenues par broyage de produit commercial ainsi que par spray pyrolyse et complètement caractérisées par FTIR, ATG/DTG, DRX, MEB et BET. Les réactions de couplage ont été activées par deux méthodes sans solvant: par broyage dans une broyeuse planétaire ou par traitement thermique sous vide. Alors qu'en UHV le couplage de l'acide 4-iodobenzoïque donne l'acide biphenyldicarboxylique, en mécanochimie nous avons obtenu l'acide benzoïque et par activation thermique l'éther dibenzoïque
Covalent coupling on metallic surfaces in UHV (Ultra High Vacuum) conditions is a new method for preparing molecular structures otherwise impossible to achieve in solution (graphene nanoribbons, 2D polymers for instance). The major challenge is now to extend these reactions from metallic to insulating surfaces, for future applications as, for instance, in molecular electronics. In particular, the coupling reaction of benzoic acid derivatives, grafted on calcite via carboxylic groups, has been demonstrated for the first time in UHV conditions. In the first part of this work, we synthesized precursor molecules for specific reactions (homocoupling of ethynes, photopolymerization, polycondensation and Ullmann reaction) on calcium carbonate in UHV conditions. In the second part of this work we extended this investigation up to the macroscale level (semi-preparative) by grafting molecules on calcium carbonate microparticles, followed by reaction activation and finally by dissolution of the substrate in order to recover the coupling products. The calcium carbonate microparticles were prepared by grinding commercial product or by spray pyrolysis and were fully characterized by FTIR, TG/DTG, XRD, SEM and BET techniques. Then, after grafting of organic reactant, the reactions were activated with two different solvent-free methods: by grinding in a planetary milling machine or by heating the samples in a furnace under vacuum. Whereas in UHV conditions, 4-iodobenzoic acid affords biphenyldicarboxylic acid, mechanochemical condition gives benzoic acid and thermal activation the dibenzoic acid ether
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13

Ye, Fei. "Ru- and Rh-catalyzed [2+2+2] cycloadditions : an access to fluorenone, 2-aminopyridine, and 1,3-dihydroisobenzofuran derivatives." Thesis, Paris 6, 2017. http://www.theses.fr/2017PA066347/document.

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Ce manuscrit traite de la mise au point d’une méthode d’accès éco-compatible à des squelettes carbocycliques et hétérocycliques, présents dans de nombreux composés d’intérêt biologique. Cette méthode met en œuvre une réaction de cycloaddition [2+2+2] catalysée par un métal de transition. Dans un premier temps, une voie d’accès à des fluorénones hautement substituées, ainsi qu’à des analogues a été développée. Cette voie utilise une réaction de cycloaddition [2+2+2] de diynes-[alpha, omega] pontés par un groupe benzoyle, avec des alcynes, en présence de RuCl3·nH2O. Dans un deuxième temps, des dérivés 2-aminopyridines diversement fonctionnalisés ont été synthétisés via une catalyse au ruthénium neutre (RuCl3·nH2O) ou cationique (Cp*Ru(CH3CN)3PF6), et ce à partir de la cycloaddition [2+2+2] de diynes et de cyanamides. Dans le cas où Cp*Ru(CH3CN)3PF6 a été utilisé comme catalyseur, une excellente régiosélectivité a été observée, ce qui a permis d’isoler une grande variété de 2-aminopyridines, dont des halopyridines, des vinylpyridines, ou des amino-aza-fluorénones. Dans une dernière partie, la cycloaddition [2+2+2] énantiosélective de triynes prochiraux avec des mono alcynes a été examinée. Elle a été conduite en utilisant un catalyseur cationique au rhodium, le complexe [Rh(cod)2]BF4/(R)-BINAP, et a permis la préparation de dérivés de 1,3-dihydroisobenzofuranes énantiomériquement enrichis, contenant un carbone quaternaire stéréogène
This manuscript focused on the development of eco-friendly and mild processes to access original carbocyclic and heterocyclic scaffolds of biological interest through transition-metal-catalyzed [2+2+2] cycloaddition reactions. Initially, an efficient and practical route for the preparation of highly substituted fluorenones and analogues via solventless RuCl3·nH2O-mediated [2+2+2] cycloaddition of benzoyl bridged [alpha, omega]-diynes and alkynes was developed. Secondly, various functionalized 2-aminopyridine derivatives were synthesized using both neutral RuCl3·nH2O and cationic Cp*Ru(CH3CN)3PF6 complexes to catalyze the [2+2+2] cycloaddition of diynes and cyanamides under solvent-free conditions. With Cp*Ru(CH3CN)3PF6 as catalyst, excellent regioselectivities were achieved to provide a wide range of 2-aminopyridines of high synthetic utility involving halopyridines, vinyl pyridines and amino-aza-fluorenones. Finally, the enantioselective rhodium-catalyzed [2+2+2] cycloaddition of prochiral triynes and monoalkynes was carried out in the presence of cationic [Rh(cod)2]BF4/(R)-BINAP complex to provide enantioenriched 1,3-dihydroisobenzofuran derivatives containing a quaternary carbon stereogenic center
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14

Krol, Michael Joseph Jr. "The Solvent-Free Synthesis of and N-Methyl-N-Alkylpiperidinium Salts and Their Anion Exchange Reactions with Dilithium Phthalocyanine." Wright State University / OhioLINK, 2013. http://rave.ohiolink.edu/etdc/view?acc_num=wright1366905299.

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15

Staleva, Plamena Krasimirova Verfasser], Carsten [Akademischer Betreuer] [Bolm, and Markus [Akademischer Betreuer] Albrecht. "Solvent-free multicomponent reactions and asymmetric transformations in solution and under mechanochemical conditions / Plamena Krasimirova Staleva ; Carsten Bolm, Markus Albrecht." Aachen : Universitätsbibliothek der RWTH Aachen, 2020. http://d-nb.info/1221373196/34.

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16

Staleva, Plamena Krasimirova [Verfasser], Carsten [Akademischer Betreuer] Bolm, and Markus [Akademischer Betreuer] Albrecht. "Solvent-free multicomponent reactions and asymmetric transformations in solution and under mechanochemical conditions / Plamena Krasimirova Staleva ; Carsten Bolm, Markus Albrecht." Aachen : Universitätsbibliothek der RWTH Aachen, 2020. http://d-nb.info/1221373196/34.

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17

Palimkar, S. S. "Novel synthetic methodologies: ionic liquid promoted friedlander heteroannulation and palladium-catalyzed copper/ligand/solvent free carbon-carbon coupling with heterocyclization reactions." Thesis(Ph.D.), CSIR-National Chemical Laboratory, Pune, 2007. http://dspace.ncl.res.in:8080/xmlui/handle/20.500.12252/2604.

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18

MAGALHAES, WELINGTON F. "Influence de parametres physico-chimiques sur les reactions du positonium en solution." Université Louis Pasteur (Strasbourg) (1971-2008), 1987. http://www.theses.fr/1987STR13218.

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19

Torregrosa, García Rubén. "Extracció reactiva de llavors oleaginoses per a la preparació de monoglicèrids." Doctoral thesis, Universitat de Lleida, 2016. http://hdl.handle.net/10803/385622.

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En aquest treball s’ha desenvolupat un mètode en dues etapes per a l’obtenció d’extractes rics en monoglicèrids a partir de llavors de soja i de sèsam. La primera etapa consisteix en una hidròlisi i esterificació directa amb glicidol i solketal dels triglicèrids continguts en les llavors, catalitzada amb miceli liofilitzat de Rhizopus oryzae en absència de solvent. La segona etapa ha estat la desprotecció del glicerol protegit en forma de 1,2-acetonid (solketal) amb catalitzadors àcids. El rendiment màxim d’obtenció de monoglicèrids a l’extracte final de reacció ha estat del 81 %, amb les següents condicions: Temps d’hidròlisi de 24 h i d’esterificació de 6 h emprant solketal, a una temperatura de reacció de de 50 °C per a la primera etapa i utilitzant com a solvent una barreja acetonitril:HCl 1M en proporció 4:1 (v/v), amb un temps de reacció de 6 h a temperatura ambient per a la segona etapa.
En este trabajo se ha desarrollado un método en dos etapas para la obtención de extractos ricos en monoglicéridos a partir de semillas de soja y de sésamo. La primera etapa consta de una hidrólisis y esterificación directa con glicidol y solketal de los triglicéridos de las semillas, catalizada con micelio liofilizado de Rhizopus oryzae en ausencia de solvente. La segunda etapa ha consistido en la desprotección del grupo 1,2-acetonido (solketal), empleando catalizadores ácidos. El rendimiento máximo de obtención de monoglicéridos en el extracto final de reacción ha sido del 81 %, empleando las siguientes condiciones: tiempo de hidrólisis de 24 h y de esterificación de 6 h utilizando solketal, a una temperatura de reacción de 50 °C para la primera etapa y utilizando como solvente una mezcla de acetonitrilo:HCl 1M en proporción 4:1 (v/v), con un tiempo de reacción de 6 h a temperatura ambiente para la segunda etapa.
In this work, a two-step method has been developed to prepare monoglyceride enriched extracts from soybean and sesame seeds. In the first step, direct extraction, hydrolysis and esterification of triglycerides from seeds is performed with glycidol and solketal. Reactions are catalyzed with lyophilized mycelium of Rhizopus oryzae in solvent-free conditions. The second step is the cleavage of solketal ring (1,2-acetonide structure) using acid catalysts. The maximum yield of monoglycerides in the two-step reaction process is 81 % using the following conditions: reaction time of 24 h for hydrolysis and 6 h for esterification using solketal, at a temperature of 50 °C in the first step and using a solvent mixture of acetonitrile:1 M HCl in 4:1 (v/v) with a reaction time of 6 h at room temperature in the second step.
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20

Kong, Yao-Zhang, and 孔堯璋. "Using Free Radical SH2 Reaction to Study the Free Radical Addition Cyclization Reactions by Substituent Effect, Solvent Effect and Stereochemistry." Thesis, 2011. http://ndltd.ncl.edu.tw/handle/85018809222472425275.

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碩士
義守大學
生物技術與化學工程研究所碩士班
99
In recent years, using the free radicals in organic synthesis becomes more important, especially the regioselectivity and stereoselectivity of the free radical cyclization reactions are highly regarded. The free radical addition cyclization reactions of t-butyl radical with asymmetric dienes, (E)-4-bromobut-2-enyl acrylate) and (N-benzyl-N-(2-(chloro methyl)allyl)acrylamide) , have been studied. The regioselectivity and stereoselectivity of the free radical addition cyclization were studies by the substituent effect which includes the polar effect and the steric effect. The structure and stereochemistry of the addition cyclization products were established and identified. The regioselectivity and stereoselectivity of the free radical addition cyclization were also studies by the solvent effect. The solvents include dimethyl sulfoxide, acetonitrile, tetrahydrofuran, and benzene.
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21

Wang, Yi-Fu, and 王義富. "Three-component Reaction : Efficient and Facile Method for the One-pot Synthesis ofα-Aminophosphonates using new Catalyst under Solvent-free Condition." Thesis, 2006. http://ndltd.ncl.edu.tw/handle/84580174679716917946.

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碩士
國立臺灣師範大學
化學系
94
α-Amino phosphonates can be synthesized by using carbonyl compounds (aldehyde or ketone)、aniline ,and triethylphosphite in the presence of the proper catalysts(Iodine,Trichloro-1,3,5-Triazine,Ceric Ammonium Nitrate,or Iron Chloride) under solvent-free condition at room temperature. The methodology can afford high yields of products and short reaction time compared to tranditional methods.
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22

"Tin (II) compounds as novel catalysts for the Kabachnik-Fields reaction: Studies in the synthesis of alpha-aminophosphonates under solvent free conditions and Synthesis of phosphonates and phosphates as reversible and irreversible inhibitors of butyrylcholinesterase." CALIFORNIA STATE UNIVERSITY, LONG BEACH, 2010. http://pqdtopen.proquest.com/#viewpdf?dispub=1472277.

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23

Budhai, Asheena. "Migration and decarbonylation reactions of group 6 organometallic complexes using solvent-free procedures." Thesis, 2008. http://hdl.handle.net/10539/5389.

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24

jiangjialong and 江佳隆. "Cycloaddition Reactions of Allylic Alcohols and Nitrile Oxides Under Solvent-Free Conditions." Thesis, 2000. http://ndltd.ncl.edu.tw/handle/98973277787234160994.

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碩士
國立中興大學
化學系
88
Isoxazoline, prepared by 1,3-dipolar cycloaddition reaction of nitrile oxide and olefin, is an important intermediate in organic synthesis. In this thesis we report our studies on the 1,3-dipolar cycloaddition reaction of benzohydroximoyl chloride and eleven different allylic alcohols under solvent-free conditions. The reaction was carried out either using focused-microwave irradiation for 20 minutes or by conventional heating for 1 h. NaHCO3 was used as the base and Aliquat 336 was used as the phase transfer catalyst. The yields were higher than those obtained previously when benzene was used as the solvent and triethylamine was used as the base. An environmentally more friendly, and more convenient process has been established for the preparation of isoxazoline.
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25

Cao, Q., Deborah E. Crawford, C. Shi, and S. L. James. "Greener dye synthesis: continuous, solvent-free synthesis of commodity perylene diimides by twin-screw extrusion." 2019. http://hdl.handle.net/10454/17622.

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Yes
A continuous, scalable, and solvent‐free method for the synthesis of various naphthalic imides and perylene diimides (PDIs) using twin‐screw extrusion (TSE) is reported. Using TSE, naphthalic imides were obtained quantitatively without the need for excess amine reactant or product purification. With good functional‐group tolerance, alkyl and benzyl amine derived PDIs (incl. commercial dyes) were obtained in 50–99 % yield. Use of K2CO3, enabled synthesis of more difficult aniline‐derived PDIs. Furthermore, an automated continuous TSE process for Pigments Black 31 and 32 is demonstrated, with a throughput rate of about 1500 g day−1, corresponding to a space time yield of about 30×103 kg m−3 day−1, which is 1–2 orders of magnitude greater than for solvent‐based batch methods. These methods provide substantial waste reductions and improved efficiency compared to conventional solvent‐based methods.
Engineering and Physical Sciences Research Council. Grant Numbers: EP/L019655/1, IAA1718-04-1117
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26

Tseng, Chao-Ming, and 曾昭明. "The Role of Solvents in Oxidative Free Radical Reaction Initiated by Manganese(Ⅲ)Acetate Between 1,4-Quinone and Carbonyl Compounds." Thesis, 2004. http://ndltd.ncl.edu.tw/handle/8nn9c9.

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碩士
國立成功大學
化學系碩博士班
92
During the past 30 years, initiated cyclization by free-radical plays an important role for synthesis of cyclic compounds.There are two methods to produce free radical. First is reduction free-radical reaction, the other is oxidative free-radical reaction. The metals used in these reactions are also different. Commercially available Mn(OAc)3•2H2O has been used for the majority of oxidative cyclizations. In this report, we chose Mn(Ⅲ)as oxidant in our oxidative free-radical reaction.   There are two parts in this report. First one is solvent effect in oxidative free-radical reaction initiated by Mn(Ⅲ)between 2-amino-1,4-naphthoquinone and 1,3-dicarbonyl compounds(eq.1, eq.2, eq.3, eq.4). The other is solvent effect in oxidative free-radical reaction initiated by Mn ( Ⅲ ) between 2-amino-1,4-naphthoquinone and carbonyl compounds(eq.5,eq.6, eq.7).
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27

Chang, Jen-Ching, and 張瑞呈. "The Role of Solvents in Oxidative Free Radical Reaction Initiated by Manganese(Ⅲ)Acetate Between 1,4-Benzoquinone and Carbonyl Compounds." Thesis, 2005. http://ndltd.ncl.edu.tw/handle/76137219915922957379.

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碩士
國立成功大學
化學系碩博士班
93
During the past 30 years, initiated cyclization by free-radical plays an important role for synthesis of cyclic compounds. There are two methods to produce free radical. First is reduction free-radical reaction, the other is oxidative free-radical reaction. The metals used in these reactions are also different. Commerci-ally available Mn(OAc)3•2H2O has been used for the majority of oxidative cyclizations. In this report, we chose Mn(III)as oxidant in our oxidative free-radical reaction. There are only one part in this report. This is solvent effect in oxidative free-radical reaction initiated by Mn(III) between 2-amino-1,4-benzoquinone and 1,3-dicarbonyl compounds.(eq 1.)
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