Some Features of Cycloalkylation Reactions of Phenol with 1-Methylcyclopentene

2021 ◽  
Vol 899 ◽  
pp. 726-732
Author(s):  
Fatma I. Gasimova ◽  
Zaur Z. Aghamali̇yev ◽  
Gulshan J. Gasanova ◽  
Chingiz K. Rasulov
Keyword(s):  
Reaction Time ◽  
Nmr Spectroscopy ◽  
Physicochemical Parameters ◽  
Molar Ratio ◽  
High Yield ◽  
Target Product ◽  
Molar Ratios ◽  
Chemical Structures ◽  
Effective Conditions ◽  
Yield Of Target Product

The present study deals with the investigation of catalytic cycloalkylation reactions of phenol with 1-methylcyclopentene. KU-23 and aluminum phenolate were used as catalysts for the process. The effect of kinetic parameters (temperature, duration, molar ratios of the initial components and the amount of catalyst) on the yield and selectivity of methylcyclopentyl phenols obtained as a result of scientific research was investigated. As a result, effective conditions were found for the production of para- and ortho-, ortho- (1-methylcyclopentyl) phenols with high yield and selectivity. It was determined that high yield of target product in the presence of phenol, 1-methylcyclopentene and catalyst KU-23, was 71.2% for phenol and selectivity for target product - 92.8% is obtained under the following conditions of cycloalkylation reaction: temperature 110°C, reaction time-5 hours, molar ratio phenol to methylcyclopentene-1 : 1, the amount of catalyst-10% according to the phenol taken. The cycloalkylation reaction of phenol with 1-methylcyclopentene in the presence of aluminum phenolate catalyst was carried out in an autoclave in a nitrogen environment and effective conditions were found: temperature 260°C, reaction time - 5 hours, molar ratio of phenol to 1-methylcyclopentene 1: 2, amount of catalyst 20% according to the phenol taken. Under these conditions, the yield of the target product is 44.3% for the phenol taken, and the selectivity is 87.6% for the target product. The chemical structures of the synthesized para- and ortho-, ortho- (1-methylcyclopentyl) phenols were confirmed by IR-, 1H and NMR spectroscopy, and physicochemical parameters were determined.

scholarly journals Synthesis of thiocol oligomer based on sodium tetrasulphide, epichlorhydrine and ammonium phosphate

2021 ◽  
pp. 32-37
Keyword(s):  
Differential Scanning Calorimetry ◽  
Reaction Time ◽  
Ir Spectroscopy ◽  
Ammonium Phosphate ◽  
Molar Ratio ◽  
Target Product ◽  
Optimal Conditions ◽  
Scanning Calorimetry ◽  
Molar Ratios ◽  
Main Component

The aim is to synthesize and study thiokol oligomer NEP-12 based on sodium tetrasulfide, epichlorohydrin and ammonium phosphate, which is intended for use as the main component of thiokol sealant. To achieve this goal, a thiokol oligomer based on sodium tetrasulfide, epichlorohydrin, and ammonium phosphate has been synthesized and investigated, and the optimal conditions for the synthesis of a thiokol oligomer have been determined. Research has been carried out on the influence of the molar ratios of the starting substances on the composition and physicochemical properties of the synthesized thiocol oligomer. 80 °C was taken as the optimum polycondensation temperature, the reaction time in this case is 1.5-2 hours, as a result, the yield of the target product reaches 94%. The thiokol oligomer with the best performance was obtained at a 1: 1: 1 molar ratio of sodium tetrasulfide, epichlorohydrin, and ammonium phosphate, respectively. Based on the results of IR spectroscopy and differential scanning calorimetry, a reaction for the formation of a thiokol oligomer is proposed.

scholarly journals Yield and Quality Characteristics of Brassica Microgreens as Affected by the NH4:NO3 Molar Ratio and Strength of the Nutrient Solution

Foods ◽  
2020 ◽  
Vol 9 (5) ◽  
pp. 677 ◽  
Author(s):  
Onofrio Davide Palmitessa ◽  
Massimiliano Renna ◽  
Pasquale Crupi ◽  
Angelo Lovece ◽  
Filomena Corbo ◽  
...  
Keyword(s):  
Nutrient Solution ◽  
Inorganic Ions ◽  
Molar Ratio ◽  
High Yield ◽  
Nitrate Content ◽  
Carotene Content ◽  
Molar Ratios ◽  
Half Strength ◽  
Nutrient Solutions ◽  
Β Carotene

Microgreens are gaining more and more interest, but little information is available on the effects of the chemical composition of the nutrient solution on the microgreen yield. In this study, three Brassica genotypes (B. oleracea var. italica, B. oleracea var. botrytis, and Brassica rapa L. subsp. sylvestris L. Janch. var. esculenta Hort) were fertigated with three modified strength Hoagland nutrient solutions (1/2, 1/4, and 1/8 strength) or with three modified half-strength Hoagland nutrient solutions with three different NH4:NO3 molar ratios (5:95, 15:85, and 25:75). Microgreen yields and content of inorganic ions, dietary fiber, proteins, α-tocopherol, and β-carotene were evaluated. Micro cauliflower showed the highest yield, as well as a higher content of mineral elements and α-tocopherol (10.4 mg 100 g−1 fresh weight (FW)) than other genotypes. The use of nutrient solution at half strength gave both a high yield (0.23 g cm−2) and a desirable seedling height. By changing the NH4:NO3 molar ratio in the nutrient solution, no differences were found on yield and growing parameters, although the highest β-carotene content (6.3 mg 100 g−1 FW) was found by using a NH4:NO3 molar ratio of 25:75. The lowest nitrate content (on average 6.8 g 100 g−1 dry weight) was found in micro broccoli and micro broccoli raab by using a nutrient solution with NH4:NO3 molar ratios of 25:75 and 5:95, respectively. Micro cauliflower fertigated with a NH4:NO3 molar ratio of 25:75 showed the highest dry matter (9.8 g 100 g−1 FW) and protein content (4.2 g 100 g−1 FW).

Degradation of herbicides (ametryn and isoproturon) during water disinfection by means of two oxidants (hypochlorite and chlorine dioxide)

1997 ◽  
Vol 35 (4) ◽  
pp. 129-136 ◽  
Author(s):  
A. Lopez ◽  
G. Mascolo ◽  
G. Tiravanti ◽  
R. Passino
Keyword(s):  
Aqueous Solution ◽  
Reaction Time ◽  
Sodium Hypochlorite ◽  
Chlorine Dioxide ◽  
Hydrolysis Product ◽  
Water Disinfection ◽  
Experimental Conditions ◽  
Molar Ratios ◽  
Chemical Structures ◽  
Opposite Trend

The paper reports the results of an investigation aimed to find out the number and the chemical structures of byproducts which form during the reactions occurring in aqueous solution between two very common disinfectants, sodium hypochlorite (NaClO) and chlorine dioxide (ClO2), and two herbicides widely used in agriculture and frequently found in groundwaters: ametryn and isoproturon. Under controlled experimental conditions [T=20°C, pH=7, reaction-time = 48h, herbicide/disinfectant molar ratios: 0.05 and 0.05×10−2], ametryn reactions with chlorine dioxide much slower than with sodium hypochlorite, whereas the opposite trend has been observed for isoproturon. In any case, however, the higher the reagents concentration the faster the reactions. As for reaction byproducts, they have been detected by HPLC and identified by HPLC-MS. In particular, ametryn (R-S-CH3) reaction with NaClO gives rise to the consecutive formation of four derivatives: the sulphoxide (R-SO-CH3), the sulphone (R-SO2-CH3), the sulphonate ester (R-O-SO2-CH3) and its hydrolysis product (R-OH). Within the fixed reaction time (48h), ametryn reaction with ClO2 forms only the sulphoxide derivative (R-SO-CH3). As for isoproturon, it reacts with both oxidants forming aromatic-ring substituted derivatives. In particular, during the reactions with NaClO and ClO2, four and two (chlorinated and/or hydroxylated) derivatives are respectively formed.

Synthesis, characterization and enzymatic degradation of copolymers of ε-caprolactone and hydroxy-fatty acids

2016 ◽  
Vol 88 (12) ◽  
pp. 1191-1201 ◽  
Author(s):  
Diana Aparaschivei ◽  
Anamaria Todea ◽  
Iulia Păuşescu ◽  
Valentin Badea ◽  
Mihai Medeleanu ◽  
...  
Keyword(s):  
Fatty Acids ◽  
Degradation Products ◽  
Hydroxy Fatty Acids ◽  
Molar Ratio ◽  
Molar Ratios ◽  
Chemical Structures ◽  
Buffer Solutions ◽  
Different Temperatures ◽  
Ft Ir ◽  
Candida Antarctica B

AbstractNew copolymers of ε-caprolactone with three hydroxy-fatty acids, 12-hydroxy stearic acid, 16-hydroxyhexadecanoic acid and ricinoleic acid, were synthesized by catalytic polyesterification. The reactions were carried out in solvent-free systems and in organic solvents as well, using tin(II) 2-ethylhexanoate as catalyst, at different temperatures and molar ratios of the comonomers. Cyclic and linear polymeric products with medium molar weight of about 2000 Da have been synthesized and their chemical structures were confirmed by FT-IR, NMR and MALDI-TOF MS analysis. The synthesis parameters were optimized and the ε-caprolactone/hydroxy acid molar ratio was set as 5:1, according to mass spectrometry results. The biodegradability of the newly synthesized polymers was studied in the presence of Candida antarctica B lipase in phosphate buffer solutions (pH=7.4), at 37°C. The weight-loss profile emphasized the degradation of the 16-hydroxyhexadecanoic acid based polymer samples at more than 50% of their initial weight in 18 days of incubation in the presence of the lipase. The composition of the degradation products was assessed using the GC-MS technique and displayed residues of the comonomers moieties.

Gold Clustering at Dimethylsulfoximine Me2S(O)NH

2000 ◽  
Vol 55 (10) ◽  
pp. 889-894 ◽  
Author(s):  
Armin Hamel ◽  
Christian Hollatz ◽  
Annette Schier ◽  
Hubert Schmidbaur
Keyword(s):  
Nitrogen Atom ◽  
Dinuclear Complex ◽  
Trinuclear Complex ◽  
Molar Ratio ◽  
High Yield ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molar Ratios ◽  
Pyramidal Configuration ◽  
Unknown Structure

Abstract Gold Clustering, Dimethylsulfoximine Polyaurated complexes of the dimethylsulfoximide anion [Me2S(O)N]- have been prepared by reacting N-trimethylsilyl-dimethylsulfoximide with [(Ph3P)Au]BF4 in various molar ratios. With one or two equivalents of the gold(I) reagent only the dinuclear complex is obtained in high yield: {[(Ph3P)Au]2NS(O)Me2}+ BF4- . With three or four equivalents only the trinuclear complex is produced: {[(Ph3P)Au]3NS(O)Me2}2+ 2 BF4- . No mono- or tetra-auration was observed, respectively. The composition of the compounds has been confirmed by analytical and spectroscopic data, and the crystal structure of the dinuclear compound has been determined by single crystal X-ray diffraction of the dichloromethane solvate. The two gold atoms are found to be coordinated to the nitrogen atom with a small Au-N-Au angle of only 92.3(3)° and a short Au-Au distance of 2.9900(5) Å. The nitrogen atom is in a distorted trigonal pyramidal configuration which allows an intramolecular SO-Au contact. For the trinuclear complex a structure with a tetracoordinate nitrogen atom [SNAU3] is proposed which is analogous to the corresponding complexes of phosphinimines R3P=NH. With the ditertiary phosphine Ph2PCH2Ch2PPh2 (dppe) a cyclic dinuclear complex (dppe)Au2[NS(0 )Me2]BF4 can be synthesized starting from (dppe)Au2Cl2. The reaction of the phosphine-rich precursor [(Ph3P)2Au]BF4 with Me3SiNS(0 )Me2 in the molar ratio 2:1 affords a binuclear complex {[(Ph3P)2Au]2NS(0 )Me2}BF4 of an as yet unknown structure

scholarly journals Comparison of homogeneous and heterogeneous catalysis for synthesis of biodiesel from M. indica oil

2011 ◽  
Vol 17 (2) ◽  
pp. 117-124 ◽  
Author(s):  
B. Singh ◽  
Faizal Bux ◽  
Y.C. Sharma
Keyword(s):  
Reaction Time ◽  
Heterogeneous Catalysis ◽  
Heterogeneous Catalyst ◽  
Reaction Temperature ◽  
Molar Ratio ◽  
High Yield ◽  
Homogeneous Catalyst ◽  
Catalyst Amount ◽  
Optimum Yield

Biodiesel was developed by transesterification of Madhuca indica oil by homogeneous and heterogeneous catalysis. KOH and CaO were taken as homogeneous and heterogeneous catalyst respectively. It was found that the homogeneous catalyst (KOH) took 1.0 h of reaction time, 6:1 methanol to oil molar ratio, 0.75 wt% of catalyst amount, 55?0.5?C reaction temperature for completion of the reaction. The heterogeneous catalyst (CaO) was found to give optimum yield in 2.5 h of reaction time at 8:1 methanol to oil molar ratio, 2.5 wt% of catalyst amount, at 65?0.5?C. A high yield (95-97%) and conversion (>96.5%) was obtained from both the catalysts. CaO was found to leach to some extent in the reactants and a biodiesel conversion of 27-28% was observed as a result of leaching.

scholarly journals SINTESIS OF 2-HIDROXY-5-ARYLALKYLACETOFENONE ОN THE BASIS OF PRODUCT OF PHENOL REACTION WITH THE COMPONENTS OF FRACTION 130-190 C PIROLYSIS PRODUCTS

2017 ◽  
Vol 60 (7) ◽  
pp. 57
Author(s):  
Emin A. Majidov ◽  
Mekhmet M. Chalyshkan ◽  
Rena Z. Bagirzade ◽  
Fuad V. Kuliev ◽  
Chingiz K. Rasulov
Keyword(s):  
Acetic Acid ◽  
Reaction Time ◽  
Solar Radiation ◽  
Physicochemical Parameters ◽  
Molar Ratio ◽  
Optimal Conditions ◽  
Unsaturated Hydrocarbons ◽  
Pyrolysis Products ◽  
Before And After ◽  
Methyl Styrene

The results of arylalkylation of phenol with components of fraction 130-190 °C of pyrolysis products in the presence of KU-23 catalyst and the influence of various parameters on the yield and selectivity of the desired product are presented. Optimal conditions for the synthesis of p-aryl-alkylphenol are found. The reaction temperature was varied from 80 to 140 °C, the reaction time was 2 to 8 hours, the molar ratio of phenol to the fraction of 130-190 °C of pyrolysis products was from 1:1 to 1:3 mol/mol, the amount of catalyst from 4 to 15 %. It was found that the interaction of phenol with FLPP in the presence of KU-23 catalyst proceeds with the formation of p-substituted arylalkylphenol. It was determined that the reaction of arylalkylation of phenol with FLPP proceeds mainly with four components of the fraction. Chromatographic studies of FLPP before and after the phenol arylalkylation reaction showed that, mainly (91.5%), unsaturated hydrocarbons enter the reaction (styrene, α-methylstyrene, vinyltoluene, indene). In this case, the concentration of styrene in the FLPP after the reaction decreases from 33.65% to 3.78%, i.e. an obtained p-aryl-alkylphenol consisted of 95.0% p-α-methylbenzylphenol. Insofar as from unsaturated hydrocarbons FLPP mainly consists of 33.65% styrene, 6.15% α-methyl-styrene, 7.02% vinyltoluene, 4.85% indene, the reaction of the alkylation going with them. It is shown that under optimal conditions, the yield of the target p-arylalkylphenol is 74.7% of the theory, and the selectivity is 92.3%. On the basis of p-arylalkylphenol and acetic acid, 2-hydroxy-5-arylalkylacetophenon was synthesized and tested as a photostabilizer of polystyrene. It is shown that under optimal conditions, the yield of the target p-arylalkylphenol is 74.7% of the theory, and the selectivity is 92.3%. Physicochemical parameters of synthesized p-arylalkylphenol and 2-hydroxy-5-arylalkylacetophenone were determined. The use of arylalkylacetophenone as an inhibitor that increases the antioxidant stability of the polystyrene, used under both thermal and solar radiation, is proposed.For citation:Majidov E.A., Chalyshkan M.M., Bagirzade R.Z., Kuliev F.V., Rasulov Ch.K. Sintesis of 2-hidroxy-5-arylalkylacetofenone оn the basis of product of phenol reaction with the components of fraction 130-190 °C pirolysis products. Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol. 2017. V. 60. N 7. P. 57-65.

scholarly journals Mixed-Metal Oxide Catalyst for Liquid Phase Benzene Alkylation

2019 ◽  
pp. 217-234
Author(s):  
M. Alhassan ◽  
U. Z. Faruq ◽  
A. Galadima
Keyword(s):  
Reaction Time ◽  
Acid Catalyst ◽  
Product Yield ◽  
Molar Ratio ◽  
Solid Catalyst ◽  
Mixed Metal Oxide ◽  
Absorption Bands ◽  
Molar Ratios ◽  
Stirred Reactor ◽  
Heterogeneous Acid Catalyst

Development of cheaper, active and more ecofriendly heterogeneous acid catalyst is a challenge mitigating the petrochemical industries. CuO-MoO3/ZrO2 solid catalyst was prepared by impregnation using suitable precursor materials supported over zirconia. Upon calcination at 450°C for 2 h and activation (by soaking in 2M H2SO4 for 30 minutes), available techniques were employed for the characterization. The available oxides and minerals in the catalyst were revealed by the XRF and XRD profiles respectively. The catalyst crystallite size (131.6nm) was obtained using the Bragg’s equation from the latter. Thermal analysis showed three weight loss stages between (49.25-152.06°C), (152.06-559.47°C) and (559.47-752.0°C ) while presence of sulphate and zirconia oxides was revealed by the FTIR analysis due to appearance of absorption bands around 1225-980cm-1 and 700-600cm-1 respectively. The catalyst (1wt%) was tested for alkylation in a continuous stirred reactor at 80°C using variable (2:1, 4:1 and 10:1) benzene to 1-decene molar ratios. The effects of reaction time and molar ratios on the selectivity, conversion and yield were determined. The alkylation results showed that the catalyst is highly selective to 1-decylbenzene as low amount of side products was obtained. The product yield and conversion increased with reaction time and benzene /1-decene molar ratio while selectivity decreased with increase in benzene /1-decene molar ratio with time.

scholarly journals PENGARUH VARIASI VARIABEL REAKSI PADA PROSES EKSTRAKSI REAKTIF MESOKARP SAWIT UNTUK MENGHASILKAN BIODIESEL

2015 ◽  
Vol 4 (4) ◽  
pp. 18-24
Author(s):  
Pascalis Novalina ◽  
Arya Josua S ◽  
Taslim ◽  
Tjahjono Herawan
Keyword(s):  
Reaction Time ◽  
Dimethyl Carbonate ◽  
Methyl Esters ◽  
Production Costs ◽  
Raw Material ◽  
Reactive Extraction ◽  
Molar Ratio ◽  
High Yield ◽  
Palm Fruit ◽  
Dialkyl Carbonates

The conventional method for the production of biodiesel needed the oil that is extracted from the biomass before it can be transesterified into fatty acid methyl esters (FAME). Reactive extraction can be used to produce biodiesel with high-yield, low production costs, reduce the reaction time and the use of reagents and co-solvents, making it easier to produce biodiesel. In this study, reactive extraction applied to produce biodiesel from palm fruit mesocarp extracted using dimethyl carbonate as a solvent and reagents, and novozym®435 as a catalyst. Methanol was replaced by dialkyl carbonates, particularly dimethyl carbonate. Dimethyl carbonate can be used as a solvent and as a reagent, so reactive extraction is very easy to apply. The parameters will be study are reaction temperature (50, 60, and 70 °C), reaction time (8, 16, 24 hours), the molar ratio of reactants (50: 1, 60: 1, 70: 1 n/n ), the concentration of novozym® 435 (5%, 10%, 15% wt).The results showed that the highest biodiesel yield can be achivied at conditions temperature of 60 °C, reaction time 24 hours, molar ratio of reactants palm mesocarp to DMC 1:60, and novozym®435 concentration of 10wt%. The results showed that the synthesis of biodiesel via reactive extraction using palm mesocarp as raw material requires a low production cost.

Coordination Behavior of tBu2PH towards [{Rh(μ-Cl)(coe)2}2] (coe = cis-cyclooctene): Crystal and Molecular Structure of [{Rh(μ-Cl)(tBu2PH)2}2]

2008 ◽  
Vol 63 (9) ◽  
pp. 1035-1039 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Peter Mayer
Keyword(s):  
Molecular Structure ◽  
Nmr Spectroscopy ◽  
Crystal And Molecular Structure ◽  
Molar Ratio ◽  
X Ray ◽  
X Ray Crystallography ◽  
Molar Ratios ◽  
H Nmr ◽  
Coordination Behavior ◽  
Independent Synthesis

The reaction of [{Rh(μ-Cl)(coe)2}2] (coe = cis-cyclooctene) with tBu2PH in different solvents in various molar ratios was investigated. Working with a molar ratio of Rh to P = 1 : 2 in heptane overnight afforded [{Rh(μ-Cl)(tBu2PH)2}2] (1) in nearly quantitative yield. Upon tuning the molar ratio (Rh/P) in the range from 1 : 2 to 1 : 0.5, 31P{1H} NMR spectroscopy indicated the formation of [(tBu2PH)2Rh(μ-Cl)2Rh(coe)2] (3) besides the complexes [{Rh(μ-Cl)(coe)(tBu2PH)}2] (cis, 2a; trans, 2b). The constitution of 3 was established by an independent synthesis mixing 1 with [{Rh(μ- Cl)(coe)2}2] or [{Rh(μ-Cl)(cod)}2] (cod = 1.4-cyclooctadiene), respectively, which also yielded [(tBu2PH)2Rh(μ-Cl)2Rh(cod)] (4). Single crystals of 1 have been analyzed by X-ray crystallography (monoclinic, Cc, Z = 8, a = 32.7375(3), b = 11.1294(1), c = 24.5134(3)Å ; β = 106.7228(4)◦; V = 8553.70(15) Å3; T = 200 (2) K).

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