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International Journal of Chemical Synthesis and Chemical Reactions International Journal of Chemical Synthesis and Chemical Reactions, focuses on the material synthesis, mass balance, kinetic analysis and other related fields of chemical synthesis process and chemical reactions. Journal accepts both experimental and theoretical papers that fall under the scope of the journal.

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Akanksha Marwah

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Deepika Bhadauria

Shrawani Verma

EDITORIAL BOARD MEMBERS Dr. A. Thirupathaiah Department of Chemistry, Chaitanya Degree & PG Colleges, Hanmakonda, Warangal, India

Dr. Ahmad Reza Massah Department of Chemistry, School of Basic Sciences, Islamic Azad University, Shahreza, Isfahan, Iran

Dr. Ajit Manharlal Bhavsar Dishman Pharmaceuticals and Chemicals Ltd., Ahmedabad, India

Dr. Anuja Chauhan Arni University, Kangra, Himachal Pradesh, India

Dr. Asif Mahmood Department of Chemical Engineering, King Saud University, Riyadh, Saudi Arabia

Dr. Avinash Sonar Department of Chemistry, VSN Arts, Commerce & Science College, Jalagaon, Mumbai, India

Dr. C Jaya Kumar Department of Chemical Engineering, A. C. Technology, Anna University, Chennai, India

Dr. Chennamsetty Subramanyam Bapatla Engineering College, Bapatla, India

Dr. Dnyaneshwar Wankhede Swami Ramanand Tirth Marathwada University, Vishnupuri, Nanded MS, India

Dr. Faiyazalam Mahmadsaiyad Shaikh Navnirman Science College, Surat, Gujarat, India

Dr. Hitesh D Patel Gujarat University, India

Kasim Mohammed Hello Al-Muthanna University, Iraq

Dr. Krishna Namdev Alasundkar Government College of Engineering, Karad Shivaji University, Kolhapur, India

Dr. Lakhwinder Singh Department of Applied Science, CGC College of Engineering, Mohali, Punjab, India

Dr. M. R. Jayapal Narasaraopeta Engineering College, Narasaraopeta, Guntur, India

Dr. Mohamed Abashar Department of Chemical Engineering, College of Engineering, King Saud University, Saudi Arabia

Dr. Mohammed Shaheer Malik CSIR-Indian Institute of Chemical Technology, India

Dr. Nandkumar M. Patil Wockhardt R & D Center, Aurangabad, India

Dr. Nitinkumar S. Shetty Department of Organic Chemistry, Manipal Institute of Technology, Manipal University (Manipal), India

Dr. Perumal Ramachandran Kongunadu College of Engineering and Technology, India

EDITORIAL BOARD MEMBERS Dr. Pradeep Kumar Rana Department of BSH, GIET, Gunupur, Odisha, India

Dr. R. P. Badoni College of Engineering Studies, University of Petroleum & Energy Studies, India

Dr. Rajeev Singh Department of Chemistry, ARSD, University of Delhi, India

Prof. Rajneesh Dutt Kaushik Gurukul Kangri University, Haridwar, Uttarakhand, India

Ramakrishna Rao Department of Chemistry, GITAM School of Technology, GITAM University, Bangalore, India

Dr. Rekha Lagarkha Department of Chemistry, Bundelkhand University, Jhansi, Uttar Pradesh, India

Dr. Saeed Khodabakhshi Nanotechnology Research Center, Research Institute of Petroleum Industry, Tehran, Iran

Dr. Sameena Bano Jamia Hamdard, India

Dr. Samson Maria Louis N Sri Ramakrishna Institute of Technology, Coimbatore, Chennai, India

Dr. Shubha Jain School of Studies in Chemistry & Biochemistry, Vikram University, Ujjain, Madhya Pradesh, India

Dr. Someshwar Dagduappa Dindulkar Department of Bioscience and Biotechnology, Konkuk University, Global hall 413, Konkuk University, 1 Hwayang-dong, Gwangin-gu, Seoul, South Korea

Dr. Sudalai Kumar S Francis Xavier Engineering College, Vannarpet Tirunelveli, Tamil Nadu, India

Dr. Suryya K Rana Dungarpur College of Engineering & Technology, Dungarpur, Rajasthan, India

Dr. Tanveer Alam University of Nizwa, Birkat Al Mouz, Nizwa, Sultanate of Oman, Oman

Dr. V. Christopher Department of Organic Chemistry, Andhra University, Visakhapatnam, India

Dr. Vajjiravel Murugesan Department of Chemistry, B. S. Abdur Rahman University, Vandalur, Chennai, Tamil Nadu, India

Prof. Velluru Sridevi Department of Chemical Engineering, A. U. College of Engineering, Andhra University, Visakhapatnam, Andhra Pradesh, India

Dr. Wilson Mbiti Njue Department of Chemistry, Kenyatta University, Nairobi Kenya, Kenya

From the Editor's Desk Dear Readers, We would like to present, with great pleasure, the inaugural volume of a new scholarly journal, International Journal of Chemical Synthesis and Chemical Reactions. This journal is part of the Applied Sciences, and is devoted to the scope of present chemical synthesis and chemical reactions issues, from theoretical aspects to application-dependent studies and the validation of emerging technologies. This new journal was planned and established to represent the growing needs of Chemical Synthesis Reactions as an emerging and increasingly vital field, now widely recognized as an integral part of scientific and technical investigations. Its mission is to become a voice of the chemical synthesis reactions Science community, addressing researchers and practitioners in this area. The core vision of International Journal of Chemical Synthesis and Chemical Reactions in Journals Pub is to propagate novel awareness and know-how for the profit of mankind ranging from the academic and professional research societies to industry practitioners in a range of topics in chemical reactions in general. Journals Pub acts as a pathfinder for the scientific community to published their papers at excellently, well-time & successfully. International Journal of Chemical Synthesis and Chemical Reactions focuses on original high-quality research in the realm of Electrosynthesis, Methods in organic synthesis, Peptide synthesis, Reaction mechanism, Kinetic analysis, Combustion, and many more. The Journal is intended as a forum for practitioners and researchers to share the techniques of chemical synthesis reactions and solutions in the area. Many scientists and researchers have contributed to the creation and the success of the chemical synthesis reactions community. We are very thankful to everybody within that community who supported the idea of creating an innovative platform. We are certain that this issue will be followed by many others, reporting new developments in the field of chemical synthesis reactions. This issue would not have been possible without the great support of the Editorial Board members, and we would like to express our sincere thanks to all of them. We would also like to express our gratitude to the editorial staff of JournalsPub, who supported us at every stage of the project. It is our hope that this fine collection of articles will be a valuable resource for chemistry readers and will stimulate further research into the vibrant area of chemical synthesis and reactions. Puneet Mehrotra Managing Director

Contents 1. Synthesis and Characterization of Cadmium-Exchanged Sodalite A.V. Borhade, S.G. Wakchaure

2. Elucidation of Synthetic Mechanism Involved in the Conversion of Zwitterionic Clonixin to Carboxamide Side-Product S. Sudalai Kumar, N. Ramkumar, D. Kodimunthiri

3. Ultrasonic Study of Binary Liquid Mixtures of Triethyl Amine With Primary Alcohols at 303.15 K Dhirendra Kumar Sharma

4. Preparation and Characterization of Ce-Si-SBA-15 Modified With Iron K.J. Rose Philo, M.A. Rahana, S. Sugunan

5. Studies on Zirconium(IV) Telluroiodate: A New Heteropolyacid Based Inorganic Ion Exchange Material Premvir Singh

International Journal of Chemical Synthesis & Chemical Reactions Vol. 2: Issue 1

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Synthesis and Characterization of Cadmium-Exchanged Sodalite A.V. Borhade1, S.G. Wakchaure2* 1

Research Centre, Department of Chemistry, HPT Arts and RYK Science College, Nashik, India 2 Department of Chemistry, PVG’s College of Engineering, Nashik, India

Abstract Cadmium derivative of chloro-sodalite has been synthesized at low temperature by hydrothermal method. The sodalite is characterized by IR, X-ray powder diffraction, and SEM. The Cd derivative was obtained by facile exchange of cadmium for sodium in chlorosodalite using a solution of cadmium nitrate in Teflon autoclaves at 100°C. The IR spectra of parent gallo silicate chloro-sodalite and cadmium-exchanged chloro-sodalites show three kinds of IR vibrations, νas (Al–O–Si) (asymmetric stretching vibrations), νs (Al–O–Si) (symmetric stretching vibrations), and δ (O–T–O) (bending vibration). Introduction of nontetrahedral cations into sodalite framework changes the IR spectra in the range of pseudolattice vibrations located at about 700–500 cm1. Parent chloro-sodalite and its cadmium derivative shows cubic symmetry in a space group P 4 3n. The crystal structures were refined by Rietveld refinement method. A considerable change is observed in cell parameters for the cadmium derivative. Cell expansion is accompanied with slight increase in T–O bond distances and T–O–T bond angles. The framework expansion takes place due to introduction of non-framework cadmium ion. The unit cell parameter (a) is 8.9502 Å for chloro-sodalite and it is found to be 9.0001 Å for cadmium sodalite. SEM pictures of cadmium derivative shows slight deposition of particles on the crystal surfaces. Keywords: cadmium, derivative, gallosilicate, sodalite

INTRODUCTION Waste water discharged by industries processing ores and concentrates of nonferrous metals are usually polluted with heavy metals, such water contains toxic heavy metals which discharged into the environment as industrial wastes causing soil and water pollution.[1] Constant trapping of heavy metal ions in the zeolite framework structure is one of the possible way of cation exchange and making them harmless. Pb+2, Cu+2 and Cd+2 are the common heavy metals which tend to accumulate in organisms and cause serious diseases and disorders.[2] They are also the commonly found ground water contaminants both at industrial and military installations. Several methods are available for removal

of dissolved heavy metals, like ion exchange, precipitation, ultrafiltration, reverse osmosis, and electrodialysis.[3–6] Activated carbon adsorption is also effective process for the removal of heavy metals at trace quantities,[7] but it is not suitable due to high cost associated with production and generation of spent carbon.[8] The use of alternative low cost material as potential sorbents for removal of heavy metals has recently been emphasized. Among various available techniques, ion exchange is considered to

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International Journal of Chemical Synthesis & Chemical Reactions Vol. 2: Issue 1

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Elucidation of Synthetic Mechanism Involved in the Conversion of Zwitterionic Clonixin to Carboxamide Side-Product S. Sudalai Kumar1,2*, N. Ramkumar2, D. Kodimunthiri1 1

Department of Science and Humanities, Francis Xavier Engineering College, SCAD Group of Institutions, Tirunelveli, Tamil Nadu, India 2 School of Chemistry, University of Hyderabad, Hyderabad, Telangana, India

Abstract N-(3-Chloro-2-methylphenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide is obtained as a byproduct during the synthesis and crystallization of Clonixin (2-(3-chloro-2methylanilino)nicotinic acid) and its polymorphs, respectively. This conversion was unexpected and it changed the usual investigation path way enabling the formation of neutral and zwitterionic polymorphs in our study on Clonixin in contrary to studies of 2-(ptolylamino) nicotinic acid investigation. The same conversion is checked in the other synthesized analogs such as 2-(phenylamino)nicotinic acid (PNA), 2(methyl(phenyl)amino)nicotinic acid (MPNA), 2-(p-tolylamino)nicotinic acid (TNA) and 2(methyl(p-tolyl)amino)nicotinic acid (MTNA) but they were all not going to any other side product formation like Clonixin. These ampholites were synthesized by the aromatic nucleophilic substitution reactions of respective aryl amines and 2-chloronicotinic acid in the presence of p-tolylsulfonic acid and pyridine in this report. However, the side product was separated from the crystallization of Clonixin in acetic acid during polymorph hunt. All other analogs were failed in giving this side product as those crystal structures of compounds were analyzed thoroughly by single crystal X-ray determination method. On comparison of this molecule with other ampholites, a new mechanism was proposed for the conversion of Clonixin to this by product in this study and the other molecules are under investigation for no conversion even though they are similar in structures.

INTRODUCTION Arylamino nicotinic acids are the organic compounds which has many medicinal applications especially they all exhibit anti-inflammatory drug properties.[1,2] Based on their importance in medical field, many arylamino nicotinic acids were synthesized by different research groups in different occasions.[3,4] Recently these molecules have some immense interest in solid state chemistry corresponding to the polymorph investigations. They have been proven in many studies that they were more prone to be polymorphic. Tetramorphs and trimorphs were reported for these molecules by Li and coworkers.[4] Some of the neutral and zwitterionic

crystal structures were also reported by Kumar and Nangia.[5] Molecular complexes for these molecules was also investigated by Kumar.[6] All these molecules fell in the category of ampholites in which they show acidic and basic behavior and exist as zwitterion in certain pH ranges. Li and coworkers[7] reported already the crystal structure of this N-(3-chloro-2-methylphenyl)-2-oxo1,2-dihydropyridine – 3 - carboxamide compound while in synthesis of Clonixin (Scheme 1). The same product was also

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International Journal of Chemical Synthesis & Chemical Reactions Vol. 2: Issue 1

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Ultrasonic Study of Binary Liquid Mixtures of Triethyl Amine With Primary Alcohols at 303.15 K Dhirendra Kumar Sharma Department of Chemistry, Bundelkhand University, Jhansi, UP, India

INTRODUCTION Most of the physical properties change whenever there is a change in the composition and structure of the liquid mixture. Then non-linear dependence of the physical–chemical properties with composition has been attributed to the size, shape, and polarity of the molecules. Ultrasonic velocity is one such property which is very important for the study of molecular interactions in solution. It gives information about the extent of interaction and some other parameters such as adiabatic compressibility and free [1] lengthy. Velocity determination of ultrasound waves enables us to study the properties of the medium, in which it travels, owing to the important of ultrasound velocity in the investigation of molecular interaction in solutions, its measurements have been carried out in the different binary liquid mixture studies in the present work.[2] ULTRASONIC AND ULTRASOUND The term, ultrasonic, refers to the science and technology dealing with acoustic waves of frequency higher than the nominal limit of audibility by the human ear. It must be called nominal limit, since it is not definable in exact terms, but only on some statistical basis, because it also depends on sex and age and varies considerably from person to person. Sound waves can be classified into three types viz. infrasonic waves, audible or sound waves, and ultrasonic waves.[3–5]

called infrasonic waves. Human ear is not sensitive to these waves. The waves are produced by large vibrating bodies such as during an earthquake. Audible or sound waves are those longitudinal waves whose frequency range produce the sensation of sound when enter into human ear. Thus, these waves are called either audible or sound waves. Audible waves are produced by vibrating bodies that includes vocal cords of humans and animals, stretched strings of musical instruments like guitar and violin, stretched membranes (e.g., drum, loudspeaker), air columns (flute), and by irregular motions of bodies (e.g., tree leaves, doors, etc.). Those audible waves which are produced by regular periodic motions of definite frequencies given pleasing effects on the ear and are called “musical sound waves.” On the other hand, those waves which reproduced by irregular non-periodic disturbances of bodies produced an irritating effect on the ear and are called “noise waves.” The longitudinal waves whose frequency lies between 20,000 and 5 × 108 Hz are “ultrasonic waves.” The ultrasonic range of full acoustic spectrum is broken down into three subsections, such as low frequency/airborne, conventional/ industrial, and high frequency/acoustic microscopy as shown in Figure 1. Human ear is not sensitive to these waves. This types of waves can be produced either by the high frequency vibration of a quartz crystal under an alternating eclectic field or by the vibration of a ferromagnetic rod

The longitudinal waves whose frequency lies below 20 Hz (cycle per second) are

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International Journal of Chemical Synthesis & Chemical Reactions Vol. 2: Issue 1

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Preparation and Characterization of Ce-Si-SBA-15 Modified With Iron K.J. Rose Philo1*, M.A. Rahana1, S. Sugunan2 1

Department of Chemistry, St. Paul’s College, Kalamassery, India Department of Applied Chemistry, Cochin University of Science and Technology, Cochin, India

Abstract Recently environmental concerns have driven the development of specialized catalysts to prevent polluting substances from being released into the environment. New technologies have improvised our understanding of catalytic functions as well as selectivity in order to save the energy and chemicals. Today, catalysis is the workhorse in the chemical industry with approximately >90% of the products produced in catalytic processes. In addition, life cannot exist without catalysis, as virtually all biochemical processes that sustain life are reliant on enzymes, nature’s own catalysts. Mixed metal oxides are multimetal multiphase oxides which typically contain one or more transition metal oxide and exhibit significant chemical and structural complexity. In recent years porous materials attract the attention of researchers and material scientists due to commercial interest in their applications in various fields especially in heterogeneous catalysis. Among the variety of catalysts, cerium oxide (CeO2) plays an important role in emerging technologies for environmental and energyrelated applications. Also many efforts have been made to investigate the pore structure of SBA-15 and utilize SBA-15 as templates for preparing nano-structured materials. Incorporation of transition metals into the SBA-15 silica framework is still a challenge in the field of mesoporous material synthesis. Only few reports are available that has successfully demonstrated the modification. Mesoporous ceria catalyst was prepared by the soft template method using the neutral surfactant hexadecyl amine (HDA). It is mixed with 15 and 20% SBA-15 prepared by surfactant assisted method using Pluronic-123. The prepared samples were modified with 10% Fe. A detailed investigation of physico-chemical characterization of the catalytic systems was performed by techniques such as wide and low angle XRD, BET surface area by sorption studies of nitrogen gas, SEM, TEM, TG/DTA and FT-IR. Keywords: hexadecyl amine, iron doping, mesoporous ceria, neutral surfactant, SBA-15

INTRODUCTION In the chemical industry and industrial research, catalysis plays an important role. Different catalysts are in constant development to fulfil economic, political and environmental demands. When using a catalyst it is possible to replace a polluting chemical reaction with a more environmentally friendly alternative. In the start only pure components were used as catalysts, but after the year 1900

multicomponent catalysts were studied and are now commonly used in the industry.[1– 8]

Typical industrial catalysts, however, consist of several components and phases. Supported catalysts play a significant role in many industrial processes. The support provides high surface area and stabilizes

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International Journal of Chemical Synthesis and Chemical Reactions Vol. 2: Issue 1

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Studies on Zirconium(IV) Telluroiodate: A New Heteropolyacid Based Inorganic Ion Exchange Material Premvir Singh* Analytical Research Laboratory, Chemistry Department, Aligarh Muslim University, Aligarh, India

Abstract Zirconium (IV) telluroiodate has been synthesized as a new inorganic cation exchanger by adding a mixture of aqueous solution of 0.1 M potassium iodate and 0.1 M sodium tellurite to aqueous solution of 0.1 M zirconium (IV) oxychloride under varying mixing ratios at pH 1. Its ion exchange capacity for Na+ was found to be 1.85 meqg1 of dry exchanger. The material has been characterized on the basis of chemical composition, FTIR, TGA, SEM and XRD. The chemical stability and thermal stability of the exchange material have also been studied. Further, various ion exchange studies such as pH titration, determination of ion exchange capacities for various metal ions and distribution behavior have been performed on this material. Keywords: cation exchanger, characterization, heteropolyacidic salt, synthesis, zirconium (IV) telluroiodate

INTRODUCTION Synthesis of new inorganic ion exchangers is always of interest. Since, they are specific in nature and can solve diverse problems of environmental and analytical chemistries.[1–3] These materials have also been employed in treatment of radioactive nuclear effluent, to remove toxic substances from aqueous effluent,[4,5] preconcentration and recovery of a number of ionic species from aqueous and nonaqueous system. These materials have also been employed in the development of chemical sensor and ion exchange membrane.[6,7] Advancement in inorganic ion exchanger is not only due to the high thermal stability and resistivity towards radiation field but also for usual selectivity for ionic species and versatility in separation. Synthetic inorganic ion exchangers based on tetravalent metal acid (TMA) salt often show much better ion exchange behavior as compared with single salt thus, such materials have been

the object of considerable studies due to their intercalation properties, higher ion exchange capacity, stability and selectivity towards certain metal ions.[8–22] In continuation of our work based on zirconium (IV) based heteropolyacid salts[23,24] ion exchangers, here we have synthesized a new heteropolyacidic salt i.e. zirconium (IV) telluroiodate, as per literature no information has been found on this material as ion exchanger. This paper presents the synthesis, characterization and ion exchange behavior of zirconium (IV) telluroiodate. EXPERIMENTAL SECTION Reagents and Chemicals Zirconium oxychloride (CDH), sodium tellurite (S. D. Fine Chem.) and potassium iodate (E Merck, India) were used for the synthesis of ion-exchangers. All other

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« « « «

¬ ¬ International Journal of Industrial Engineering

Manufacturing International Journal of Mechanical Dynamics and Analysis International Journal of Fracture and damage Mechanics International Journal of Structural Mechanics and Finite Elements

and Design ¬ International Journal of Manufacturing and

Materials Processing ¬ International Journal of Mechanical Handling and

Automation 5 more...

Electronics and Telecommunication « International Journal of Radio Frequency Design « International Journal of VLSI Design and Technology « International Journal of Embedded Systems and Emerging

Technologies « International Journal of Digital Electronics « International Journal of Digital Communication and Analog

Chemical Engineering « International Journal of Renewable Energy and its

Commercialization « International Journal of Environmental Chemistry « International Journal of Agrochemistry « International Journal of Prevention and Control of Industrial

Pollution

5 more...

Signals

1 more...

Planning « International Journal of Architecture and Infrastructure

Planning « International Journal of Rural and Regional Planning

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Development

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Electrical Engineering

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Nursing

Material Sciences and Engineering

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Biotechnology « International Journal of Industrial Biotechnology and « « « «

Jan – June 2016

« International Journal of Town Planning and Management

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IJCSCR

Civil Engineering

Architecture « International Journal of Housing and Human Settlement

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International Journal of Chemical Synthesis and Chemical Reactions

Nanotechnology « International Journal of Applied Nanotechnology « International Journal of Nanomaterials and Nanostructures « International Journals of Nanobiotechnology

Chemistry

Physics « International Journal of Solid State Materials « International Journal of Optical Sciences