A comparative study of microwave versus conventional synthesis of lead phthalocyanine complexes

2005 ◽  
Vol 09 (12) ◽  
pp. 872-879 ◽  
Author(s):  
B. Narayana Achar ◽  
T. Manjappa Mohan Kumar ◽  
K. Sannegowda Lokesh
Keyword(s):  
Ir Spectroscopy ◽  
Microwave Irradiation ◽  
Conventional Heating ◽  
High Yield ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dry Conditions ◽  
Uv Visible ◽  
First Time ◽  
Very High

Lead(II) phthalocyanine (PbPc); lead(II) tetranitrophthalocyanine (PbTNP) and lead(II) tetraaminophthalocyanine (PbTAP) were synthesized in pure state by microwave irradiation and conventional heating methods. The procedures for their synthesis by the microwave technique are standardized and reported for the first time. PbPc and PbTNP were synthesized in dry conditions and PbTAP complex was synthesized in aqueous medium. All the compounds are obtained in very high yield (~90%). The synthesized complexes are characterized with respect to elemental analysis, UV-visible, IR-spectroscopy and X-ray diffraction study. The microwave methods are advantageous over the conventional method of synthesis with respect to higher yield, rapidity and simplicity.

scholarly journals Hydrothermal Synthesis of Sb2S3Nanorods Using Iodine via Redox Mechanism

2011 ◽  
Vol 2011 ◽  
pp. 1-5 ◽  
Author(s):  
Abdolali Alemi ◽  
Sang Woo Joo ◽  
Younes Hanifehpour ◽  
Aliakbar Khandar ◽  
Ali Morsali ◽  
...  
Keyword(s):  
Elemental Sulfur ◽  
Orthorhombic Phase ◽  
Blue Shift ◽  
Atomic Ratio ◽  
High Yield ◽  
X Ray Diffraction ◽  
X Ray ◽  
Spectrometry Analysis ◽  
Pl Emission ◽  
First Time

Crystalline antimony sulfide (Sb2S3) with nanorods morphology was successfully prepared via hydrothermal method by the reaction of elemental sulfur, antimony, and iodine as starting materials with high yield at 180∘C for 24 h. Using oxidation reagent like iodine as an initiator of redox reaction to prepare Sb2S3is reported for first time. The powder X-ray diffraction pattern shows the Sb2S3crystals belong to the orthorhombic phase with calculated lattice parameters,a=1.120 nm,b=1.128 nm, andc=0.383 nm. The quantification of energy-dispersive X-ray spectrometry analysis peaks gives an atomic ratio of 2 : 3 for Sb : S. TEM and SEM studies reveal the appearance of the as-prepared Sb2S3is rodlike which is composed of nanorods with the typical width of 50–140 nm and length of up to 4 μm. The PL emission indicates that band gap of Sb2S3is around 2.50 ev, indicating a considerable blue shift relative to the bulk. A formation mechanism of Sb2S3nanostructure is proposed.

scholarly journals Accelerated syntheses of amine-bis(phenol) ligands in polyethylene glycol or “on water” under microwave irradiation

2008 ◽  
Vol 86 (5) ◽  
pp. 435-443 ◽  
Author(s):  
Francesca M Kerton ◽  
Stacey Holloway ◽  
Angela Power ◽  
R Graeme Soper ◽  
Kristina Sheridan ◽  
...  
Keyword(s):  
Polyethylene Glycol ◽  
Microwave Irradiation ◽  
Hydrophobic Effect ◽  
High Yield ◽  
Microwave Assisted Synthesis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Microwave Assisted ◽  
Mannich Condensation ◽  
Time And Energy

Pure amine-bis(phenol) ligands are readily accessible in high yield, often >90%, when the Mannich condensation reactions are performed “on water” or in poly(ethyleneglycol) (PEG). Microwave-assisted synthesis dramatically reduces the time and energy required to prepare these molecules, typically from 24 h to 5 min. The approach seems to be widely applicable (7 amines and 5 phenols were tested to yield a diverse set of bis(phenol) ligands). Significant improvements in yield were observed for ligands derived from di-tert-amyl and di-tert-butyl phenols, possibly resulting from a hydrophobic effect. Single crystal X-ray diffraction data for the ligand derived from p-cresol and N,N′-dimethylethylenediamine is reported.Key words: amine-phenol, Mannich condensation, on water, microwave, ligand, high-throughput.

Microwave Irradiation Synthesis of Sb2S3 and its Optical Characteristic

2016 ◽  
Vol 839 ◽  
pp. 136-141
Author(s):  
Arrak Klinbumrung ◽  
Chalermchai Pilapong ◽  
Tawat Suriwong
Keyword(s):  
Electron Microscopy ◽  
Microwave Irradiation ◽  
Optical Characteristic ◽  
Hydroxyethyl Cellulose ◽  
X Ray Diffraction ◽  
Energy Band Gap ◽  
Visible Spectroscopy ◽  
X Ray ◽  
Uv Visible ◽  
Scanning Electron

Antimony sulfide (Sb2S3) nanostructure was synthesized using a 600 W microwave irradiation technique. The precursors including Sb(CH3CO2)3 and Na2S2O3.5H2O were dissolved into 50 mL ethylene glycol (EG) solution with containing 0 and 1 g of hydroxyethyl cellulose (HEC). Phase, morphology and optical properties of the as-synthesized products were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-visible spectroscopy and photoluminescence (PL). Energy band gap of Sb2S3 nanostructure exhibits the value of 1.90 and 2.06 eV for synthesizing condition with and without HEC containing, respectively.

Carbacylamidophosphates: Synthesis, Properties, and Structure of Dimorfolido-N-trichloroacetylphosphorylamide

1998 ◽  
Vol 53 (4) ◽  
pp. 481-484 ◽  
Author(s):  
Vladimir A Ovchynnikov ◽  
Vladimir M Amirkhanov ◽  
Taras P Timoshenko ◽  
Tadeusz Glowiak ◽  
Henryk Kozlowskib
Keyword(s):  
Ir Spectroscopy ◽  
Hydrogen Bonds ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Synthesis Properties ◽  
First Time ◽  
Centrosymmetric Dimers ◽  
Ir Bands

Abstract Dimorpholido-N-trichloroacetylphosphorylamide: CCl3C(O)NHP(O)[N(CH2CH2)2O]2 [HL] and its sodium [NaL] and morpholine [HN(CH2-CH2)2O•HL] salts were synthesized for the first time. The compounds were studied by IR spectroscopy and assignments of the characteristic IR bands have been made. The structure of [HL] was determined by X-ray diffraction. Crystals are monoclinic, a = 11.412(2) Å, b = 16.056(3) Å, c = 9.622(2) Å, β = 108.55(3)°, space group P21/c; Z = 4. The refinement of the structure converged at R = 0.066. The molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups.

Azide und Cyanamide – ähnlich und doch anders/Azides and Cyanamides – Similar and Yet Different

2003 ◽  
Vol 58 (11) ◽  
pp. 1097-1104 ◽  
Author(s):  
Olaf Reckeweg ◽  
Arndt Simon
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystals ◽  
Crystal Structures ◽  
Spectroscopic Data ◽  
Structural Features ◽  
X Ray Diffraction ◽  
X Ray ◽  
First Time ◽  
Raman And Ir Spectroscopy

Abstract The crystal structures of LiN3*H2O (P63/mcm (No. 193), Z = 6; 924.01(13); 560.06(7) pm); NH4N3 (Pmna (No. 53), Z =4; a=889.78(18), b=380,67(8), c=867.35(17) pm); Ca(N3)2 (Fddd (No. 70), Z = 8; a=595.4(2), b=1103.6(5), c=1133.1(6) pm), Sr(N3)2 (Fddd (No. 70), Z =8; a= 612.02(9), b = 1154.60(18), c = 1182.62(15) pm); Ba(N3)2 (P21/m (No. 11), Z = 2; a = 544.8(1), b = 439.9(1), c = 961.3(2) pm, β = 99.64(3)°) and TlN3 (I4/mcm (No. 140), Z = 2; 618.96(9); 732.71(15) pm) have been either determined for the first time or redetermined by X-ray diffraction on single crystals. The afore mentioned compounds, AN3 (A = Na, K, Rb, Cs), M(N3)2 · 2.5 H2O (M = Mg, Zn) and the cyanamides Li2CN2, CdCN2 and CuCN2 were investigated by Raman and IR spectroscopy (KBr technique). Structural features and spectroscopic data of azides and cyanamides from this work and from literature are listed and compared.

scholarly journals Synthesis of β-SiC Fine Fibers by the Forcespinning Method with Microwave Irradiation

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Alfonso Salinas ◽  
Maricela Lizcano ◽  
Karen Lozano
Keyword(s):  
Microwave Irradiation ◽  
Fiber Composite ◽  
Processing Parameters ◽  
Fiber Spinning ◽  
High Yield ◽  
X Ray Diffraction ◽  
Fiber Mats ◽  
X Ray ◽  
Fine Fiber ◽  
Energy Processing

A rapid method for synthesizing β-silicon carbide (β-SiC) fine fiber composite has been achieved by combining forcespinning technology with microwave energy processing. β-SiC has applications as composite reinforcements, refractory filtration systems, and other high temperature applications given their properties such as low density, oxidation resistance, thermal stability, and wear resistance. Nonwoven fine fiber mats were prepared through a solution based method using polystyrene (PS) and polycarbomethylsilane (PCmS) as the precursor materials. The fiber spinning was performed under different parameters to obtain high yield, fiber homogeneity, and small diameters. The spinning was carried out under controlled nitrogen environment to control and reduce oxygen content. Characterization was conducted using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The results show high yield, long continuous bead-free nonwoven fine fibers with diameters ranging from 270 nm to 2 µm depending on the selected processing parameters. The fine fiber mats show formation of highly crystalline β-SiC fine fiber after microwave irradiation.

scholarly journals Synthesis and characterization of the cyanobenzene-ethylenedithio-TTF donor

2015 ◽  
Vol 11 ◽  
pp. 951-956 ◽  
Author(s):  
Sandrina Oliveira ◽  
Dulce Belo ◽  
Isabel Cordeiro Santos ◽  
Sandra Rabaça ◽  
Manuel Almeida
Keyword(s):  
Coupling Reaction ◽  
Cross Coupling ◽  
Triethyl Phosphite ◽  
High Yield ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cross Coupling Reaction ◽  
Uv Visible

A dissymmetric TTF-type electron donor, cyanobenzene-ethylenedithio-tetrathiafulvalene (CNB-EDT-TTF), was obtained in high yield, by a cross-coupling reaction with triethyl phosphite between 2-thioxobenzo[d][1,3]dithiole-5-carbonitrile and 5,6-dihydro-[1,3]dithiolo[4,5-b][1,4]dithiin-2-one. This new donor was characterized namely by single crystal X-ray diffraction, cyclic voltammetry, NMR, UV-visible and IR spectroscopy.

scholarly journals Synthesis of Energetic 7-Nitro-3,5-dihydro-4H-pyrazolo[4,3-d][1,2,3]triazin-4-one Based on a Novel Hofmann-Type Rearrangement

Molecules ◽  
2021 ◽  
Vol 26 (23) ◽  
pp. 7319
Author(s):  
Fu-Qiang Bi ◽  
Yi-Fen Luo ◽  
Jun-Lin Zhang ◽  
Huan Huo ◽  
Bo-Zhou Wang
Keyword(s):  
Differential Scanning Calorimetry ◽  
Ir Spectroscopy ◽  
Organic Synthesis ◽  
Energetic Materials ◽  
Detonation Properties ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Calculation Results ◽  
First Time

Rearrangement reactions are efficient strategies in organic synthesis and contribute enormously to the development of energetic materials. Here, we report on the preparation of a fused energetic structure of 7-nitro-3,5-dihydro-4H-pyrazolo[4,3-d][1,2,3]triazin-4-one (NPTO) based on a novel Hofmann-type rearrangement. The 1,2,3-triazine unit was introduced into the fused bicyclic skeleton from a pyrazole unit for the first time. The new compound of NPTO was fully characterized using multinuclear NMR and IR spectroscopy, elemental analysis as well as X-ray diffraction studies. The thermal behaviors and detonation properties of NPTO were investigated through a differential scanning calorimetry (DSC-TG) approach and EXPLO5 program-based calculations, respectively. The calculation results showed similar detonation performances between NPTO and the energetic materials of DNPP and ANPP, indicating that NPTO has a good application perspective in insensitive explosives and propellants.

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