Titanium-Catalyzed [4+2] and [6+2] Cycloadditions of 1,4-Bis(trimethylsilyl)buta-1,3-diyne

1996 ◽  
Vol 61 (12) ◽  
pp. 1722-1728 ◽  
Author(s):  
Jan-Willem F. Kaagman ◽  
Marco Rep ◽  
Michal Horáček ◽  
Petr Sedmera ◽  
Jiří Čejka ◽  
...  
Keyword(s):  
Molar Ratio ◽  
Initial Molar Ratio

The (C2H5)2AlCl/TiCl4 catalyst induces the [4+2] cycloaddition of butadiene or the [6+2] cycloaddition of 1,3,5-cycloheptatriene (CHT) to individual acetylenic moieties of 1,4-bis(trimethylsilyl)buta-1,3-diyne (BSD). Heating of the 2:1 butadiene adduct, bis(2-trimethylsilylcyclohexa-1,4-dien-1-yl), to 250 °C yields 2,2'-bis(trimethylsilyl)biphenyl. The 1:1 adduct of BSD with CHT, 7-trimethylsilyl-8-trimethylsilylethynylbicyclo[4.2.1]nona-2,4-diene, is obtained as virtually the only product if the initial molar ratio CHT : BD equal to 1.86 is used.

scholarly journals Investigation of propylene carbonate synthesis regularities by the interaction of propylene glycol with carbamide

2020 ◽  
Vol 15 (1) ◽  
pp. 55-61
Author(s):  
A. V. Sulimov ◽  
A. V. Ovcharova ◽  
G. M. Kravchenko ◽  
Yu. K. Sulimova
Keyword(s):  
Propylene Glycol ◽  
Propylene Carbonate ◽  
Residence Time ◽  
Zinc Acetate ◽  
Batch Reactor ◽  
Molar Ratio ◽  
High Yield ◽  
Gas Liquid Chromatography ◽  
Cyclic Carbonates ◽  
Initial Molar Ratio

Objectives. Cyclic carbonates are important products of organic synthesis, which are widely used as solvents, catalysts, and reagents for the production of various compounds (in particular, urethane-containing polymers) by the non-isocyanate method. The process of carbamide alcoholysis with polybasic alcohols is a promising method for the synthesis of cyclic carbonates. The purpose of this study is to determine the reaction conditions for the interaction of propylene glycol with carbamide in the presence of zinc acetate as a catalyst.Methods. We conducted experiments to study the synthesis of propylene carbonate in a batch laboratory apparatus. Moreover, we analyzed the starting reagents and final products using gas–liquid chromatography.Results. We studied the synthesis of propylene carbonate by carbamide alcoholysis with propylene glycol in the presence of a catalyst (zinc acetate) by varying the following parameters: initial molar ratio of propylene glycol/carbamide = (0.5–5):1, synthesis temperature 130–190°С, reagent residence time in the reactor 0.5–4 h, and the catalyst amount in the reaction mixture 0–1.5 wt %.Conclusions. We determined the technological parameters of propylene carbonate synthesis in a batch reactor. Moreover, we showed that the process allowed the production of propylene carbonate with a sufficiently high yield of 80%—at the initial molar ratio of propylene glycol/ carbamide = 3:1, temperature 170°C, and residence time 2 h.

Identification of Phosphate Precipitates from Wastewater Digested Liquor

2015 ◽  
Vol 1087 ◽  
pp. 262-266
Author(s):  
Newati Wid ◽  
Nigel Horan
Keyword(s):  
Calcium Ion ◽  
Molar Ratio ◽  
High Concentration ◽  
Xrd Pattern ◽  
Soil Conditioner ◽  
Edx Analysis ◽  
Initial Molar Ratio ◽  
Molar Ratios ◽  
Phosphate Compound ◽  
Edx Analyses

The XRD and EDX analyses were used to identify the type of phosphate precipitate from anaerobically digested liquor of wastewater screenings. The measurements confirmed that the main phosphate compound produced from the experiments was CaCO3 and HA when the Mg:P molar ratios were 1.56:1 and 2:1, respectively. The precipitation at 1.56:1 was the initial molar ratio without chemical amendment, whereas 2:1 was carried out by chemical amendment. The results indicate that the presence of foreign ions such as calcium ion in high concentration may affect the formation of phosphate precipitates. This study shows that precipitation at 2:1 is suitable to recover phosphorus from wastewater digested liquor in the form of HA, as proved by the XRD pattern and further supported by EDX analysis. According to previous studies, the phosphate precipitate has a potential as a fertiliser or soil conditioner that can be used for agricultural purpose.

FeCo nanoalloys embedded in nitrogen-doped carbon nanosheets/bamboo-like carbon nanotubes for the oxygen reduction reaction

2021 ◽  
Vol 8 (1) ◽  
pp. 109-121
Author(s):  
Xiao-Wei Song ◽  
Shuwei Zhang ◽  
Haihong Zhong ◽  
Yuan Gao ◽  
Luis A. Estudillo-Wong ◽  
...  
Keyword(s):  
Carbon Nanotubes ◽  
Oxygen Reduction Reaction ◽  
Oxygen Reduction ◽  
Reduction Reaction ◽  
Molar Ratio ◽  
Carbon Nanosheets ◽  
Nitrogen Doped ◽  
Initial Molar Ratio ◽  
Nitrogen Doped Carbon

Herein, FeCo bimetallic organic frameworks (MOFs) with different compositions were fabricated by controlling the initial molar ratio of Fe3+/Co2+ ions.

scholarly journals Influence of the Mixing Ways of Reactants on ZnO Morphology

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Lining Yang ◽  
Lan Xiang
Keyword(s):  
Thermodynamic Analysis ◽  
Room Temperature ◽  
Molar Ratio ◽  
Solution Composition ◽  
Initial Molar Ratio ◽  
Zno Particles

ZnO particles with various morphologies were synthesized by mixing ZnSO4and NaOH solutions at 25°C followed by aging of the suspensions at 40–80°C for 2.0 h, keeping the initial molar ratio of Zn2+to OH−at 1 : 4. ZnO irregular plates were prepared by adding NaOH to ZnSO4whileε-Zn(OH)2rhombic particles were produced using the opposite mixing way. After aging of the slurries at 80°C for 2.0 h, the ZnO plates were kept stable while theε-Zn(OH)2rhombic particles were converted to ZnO whiskers with a length of 1.0–4.0 μm and a diameter of 0.03–0.3 μm. Thermodynamic analysis indicated that the formation of the Zn-bearing precipitates (ZnO orε-Zn(OH)2) at room temperature was connected closely with the solution composition.

scholarly journals Telomerization of 3,3,3-Trifluoroprop-1-ene and Functionalization of Its Telomers

2008 ◽  
Vol 73 (12) ◽  
pp. 1747-1763 ◽  
Author(s):  
George K. Kostov ◽  
Bruno Améduri ◽  
Stephan Brandstadter
Keyword(s):  
Nmr Spectroscopy ◽  
Reaction Temperature ◽  
Molar Ratio ◽  
Allyl Acetate ◽  
Initial Molar Ratio ◽  
The Third ◽  
Single Isomer ◽  
Butyl Peroxide ◽  
Selective Formation ◽  
C Nmr

The synthesis of four 3,3,3-trifluoroprop-1-ene telomers (RF(C3H3F3)nI, n = 1, 2, RF = n-C6F13- or (CF3)2CF-) and their allyl derivatives RF(C3H3F3)nCH2CH=CH2 are presented. The allyl telomers were prepared by a three-step reaction. The first step involved the thermal and peroxide-induced bulk telomerization of 3,3,3-trifluoroprop-1-ene (TFP) with heptafluoro-2-iodopropane or tridecafluoro-6-iodohexane leading to monoadduct and diadduct, the ratio of which depends on the R0 = [RFI]0/[TFP]0 initial molar ratio and the reaction temperature. The amount of monoadduct increased up to 50-60% and of the diadduct to 25-30% at temperatures up to 180 °C (thermal-initiated) and 150 °C (initiated with di-tert-butyl peroxide, DTBP), R0 up to 1.5. It was observed that the addition of the (CF3)2CF• radical onto the =CH2 of TFP was regioselective leading to selective formation of a single isomer in contrast to the addition of the n-C6F13• radical. Then, the telomers reacted with allyl acetate yielding RF(C3H3F3)nCH2CH(I)CH2OCOCH3 (n = 1, 2) in 50-80% yields. The third step consisted of a deiododeacetatization of these iodoacetates into RF(C3H3F3)nCH2-CH=CH2 (C,n) giving 50-80% yields. All the intermediates were characterized by 1H, 19F and products by 13C NMR spectroscopy.

Lipid Polymorphism and Virus-Membrane Fusion as Observed in Vitrified Thin Films by Cryo-Electron Microscopy

1990 ◽  
Vol 48 (1) ◽  
pp. 492-493
Author(s):  
P.M. Frederik ◽  
K.N.J. Burger ◽  
M.C.A. Stuart ◽  
A.J. Verkleij
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Membrane Fusion ◽  
Film Formation ◽  
Molar Ratio ◽  
Influenza B ◽  
Complex Structures ◽  
Type Ii ◽  
Suspended Material ◽  
Cryo Electron Microscopy

Cellular membranes are often composed of phospholipid mixtures in which one or more components have a tendency to adopt a type II non-bilayer lipid structure such as the inverted hexagonal (H||) phase. The formation of a type II non-bilayer intermediate, the inverted lipid micel is proposed as the initial step in membrane fusion (Verkleij 1984, Siegel, 1986). In the various forms of cellular transport mediated by carrier vesicles (e.g. exocytosis, endocytosis) the regulation of membrane fusion, and hence of inverted lipid micel formation, is of vital importance.We studied the phase behaviour of simple and complex lipid mixtures by cryo-electron microscopy to gain more insight in the ultrastructure of different lipid phases (e.g. Pβ’, Lα, H||) and in the complex membrane structures arising after Lα < - > H|| phase changes (e.g. isotropic, cubic). To prepare hydrated thin films a 700 mesh hexagonal grid (without supporting film) was dipped into and withdrawn from a liposome suspension. The excess fluid was blotted against filter paper and the thin films that form between the bars of the specimen grid were immediately (within 1 second) vitrified by plunging of the carrier grids into ethane cooled to its melting point by liquid nitrogen (Dubochet et al., 1982). Surface active molecules such as phospholipids play an important role in the formation and thinning of these aqueous thin films (Frederik et al., 1989). The formation of two interfacial layers at the air-water interfaces requires transport of surface molecules from the suspension as well as the orientation of these molecules at the interfaces. During the spontaneous thinning of the film the interfaces approach each other, initially driven by capillary forces later by Van der Waals attraction. The process of thinning results in the sorting by size of the suspended material and is also accompanied by a loss of water from the thinner parts of the film. This loss of water may result in the concentration and eventually in partial dehydration of suspended material even if thin films are vitrified within 1 sec after their formation. Film formation and vitrification were initiated at temperatures between 20-60°C by placing die equipment in an incubator provided widi port holes for the necessary manipulations. Unilamellar vesicles were made from dipalmitoyl phosphatidyl choline (DPPC) by an extrusion method and showed a smooth (Lα) or a rippled (PB’.) structure depending on the temperature of the suspensions and the temperature of film formation (50°C resp. 39°C) prior to vitrification. The thermotropic phases of hydrated phospholipids are thus faithfully preserved in vitrified thin films (fig. a,b). Complex structures arose when mixtures of dioleoylphosphatidylethanol-amine (DOPE), dioleoylphosphatidylcholine (DOPC) and cholesterol (molar ratio 3/1/2) are heated and used for thin film formation. The tendency of DOPE to adopt the H|| phase is responsible for the formation of complex structures in this lipid mixture. Isotropic and cubic areas (fig. c,d) having a bilayer structure are found in coexistence with H|| cylinders (fig. e). The formation of interlamellar attachments (ILA’s) as observed in isotropic and cubic structures is also thought to be of importance in biological fusion events. Therefore the study of the fusion activity of influenza B virus with liposomes (DOPE/DOPC/cholesterol/ganglioside in a molar ratio 1/1/2/0.2) was initiated. At neutral pH only adsorption of virus to liposomes was observed whereas 2 minutes after a drop in pH (7.4 - > 5.4) fusion between virus and liposome membranes was demonstrated (fig. f). The micrographs illustrate the exciting potential of cryo-electron microscopy to study lipid-lipid and lipid-protein interactions in hydrated specimens.

A New Method for Plasminogen Standardization

1968 ◽  
Vol 20 (03/04) ◽  
pp. 548-554
Author(s):  
J Gajewski ◽  
G Markus
Keyword(s):  
Proteolytic Activity ◽  
Specific Activity ◽  
Molar Ratio ◽  
Sharp Transition ◽  
Equivalence Point ◽  
Constant Amount ◽  
Residual Level ◽  
Activity Measurements ◽  
Complete Saturation ◽  
Human Plasminogen

SummaryA method for the standardization of human plasminogen is proposed, based on the stoichiometric interaction between plasminogen and streptokinase, resulting in inhibition of proteolytic activity. Activation of a constant amount of plasminogen with increasing amounts of streptokinase yields linearly decreasing activities, as a function of streptokinase, with a sharp transition to a constant residual level. The point of transition corresponds to complete saturation of plasmin with streptokinase in a 1:1 molar ratio, and is therefore a measure of the amount of plasminogen present initially, in terms of streptokinase equivalents. The equivalence point is independent of the kind of protein substrate used, buffer, pH, length of digestion and, within limits, temperature. The method, therefore, is not subject to the variations commonly encountered in the usual determination based on specific activity measurements.

Fungicidal and Bactericidal Activity of the Alkyl-Substituted Guanidine-Containing Oligomers

2020 ◽  
Vol 82 (6) ◽  
pp. 54-63
Author(s):  
M.Ya. Vortman ◽  
◽  
Yu.B. Pysmenna ◽  
A.I. Chuenko ◽  
D.R. Abdulina ◽  
...  
Keyword(s):  
Heterotrophic Bacteria ◽  
Trichoderma Viride ◽  
Rhodococcus Erythropolis ◽  
Biological Action ◽  
Molar Ratio ◽  
Diffusion Method ◽  
Klebsiella Pneumonia ◽  
Alkyl Bromides ◽  
Base Form ◽  
Two Stages

Biocides are widely used in medicine and various industries to protect against a number of harmful microorganisms. Organic quaternary ammonium and guanidine-containing compounds, the biological action of which is based on membrane-toxic properties, are used as bactericidal preparations. The aim of this work was to study the bactericidal and fungicidal activities of the synthesized oligomeric alkylsubstituted guanidinium bromides with different radicals -C3H7, -C7H15, -C10H21, against different isolates of heterotrophic bacteria and microscopic fungi. Methods. The synthesis of alkyl-substituted guanidiniumcontaining oligomers was performed in two stages. In the first stage, alkyl-substituted guanidine was obtained by the reaction of guanidine, previously converted by alkali from the salt form to the base form by the base and alkyl bromides (Alk=-C3H7 (propyl), -C7H15 (heptyl), -C10H21 (decyl)) in methanol at a temperature of 50°C and a molar ratio of 1:1. The second carried out the reaction between aromatic oligoepoxide DER-331 and alkyl-substituted guanidine in methanol at a temperature of 50°C for 2–3 hours and a molar ratio of 1:2. Bacteria were grown on meat-peptone agar for 48 hours at a temperature of 28±2°С. Test cultures of micromycetes were cultured on agar beer wort (6°B), incubated for 14 days in a thermostat at a temperature of 28±2°C. Antimicrobial activity of newly synthesized alkyl-substituted guanidinium-containing oligomers was determined by standard disco-diffusion method (method of disks on agar) and fungicidal activity was determined by the method of holes in agar. Results. Oligomeric alkylsubstituted guanidinium bromides with different radicals composed -C3H7, -C7H15, -C10H21- synthesized by the reaction of guanidine alkyl bromides with aromatic oligoepoxydes. It was found that alkyl-substituted guanidinium-containing oligomers at a concentration of 1–3% inhibited the growth of Escherichia coli 475, Pseudomonas aeruginosa 465, Klebsiella pneumonia 479, Pseudomonas pseudoalcaligenes 109, Staphylococcus aureus 451, E. faecalis 422, Rhodococcus erythropolis 102, Bacillus subtilis 138 and most of the studied micromycetes – Aureobasidium pullulans F-41430, Paecilomyces variotii F-41432, Penicillium funiculosum F-41435, Penicillium ochrochloron F-41431, Scopulariopsis brevicaulis F-41434, Trichoderma viride F-41437, Candida albicans F-41441, Aspergillus flavus F-41442, Aspergillus niger F-41448, Penicillium sp. F-41447. Conclusions. Antimicrobial and fungicidal properties significantly depend on the length of the alkyl radical, with increasing of its length the diameter of the zone of bacterial and micromycetes growth retardation increases.10.15407/microbiolj82.06.054

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