• Title/Summary/Keyword: N,N-dimethylformamide

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Microwave Assisted Rapid Synthesis of Novel Optically Active Poly(amide-imide)s Based on N-Trimellitylimido-L-Leucine Diacid Chloride and Hydantoin Derivatives

  • Faghihi, Khalil
    • Macromolecular Research
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    • v.12 no.3
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    • pp.258-262
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    • 2004
  • We have developed facile and rapid polycondensation reactions of N-trimellitylimido-L-leucine diacid chloride 1 with eight different derivatives of hydantoin compounds 2a-h, in the presence of a small amount of a polar organic medium, such as Ο-cresol, by using a domestic microwave oven. The polycondensation reactions proceeded rapidly-they were complete within 7-9 min-to produce a series of novel optically active poly(amide-imide)s (3a-h) in high yield with inherent viscosities of 0.33-0.51 dL/g. We characterized the resulting poly(amide-imide)s by elemental analysis, thermal gravimetric analysis (DSC, TGA, and DTG), and FTIR spectroscopy, and by measuring their viscosities, specific rotations, and solubilities. All of the polymers were soluble at room temperature in polar solvents such as N ,N-dimethylacetamide, N,N-dimethylformamide, dimethylsulfoxide, tetrahydrofuran, and N-methyl-2-pyrrolidone.

Study the Electrochemical Reduction of Some Triazines in N,N-Dimethylformamide at Glassy Carbon Electrode

  • Fotouhi, L.;Farzinnegad, N.;Heravi, M.M.;Khaleghi, Sh.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.12
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    • pp.1751-1756
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    • 2003
  • An electrochemical study related to the electroreduction of 4-amino-6-methyl-3-thio-1,2,4-triazin-5-one(I), 6-methyl-3-thio-1,2,4-triazin-5-one(II), and 2,4-dimetoxy-6-methyl-1,3,5-triazine(III) in dimethylformamide at glassy carbon electrode has been performed. A variety of electrochemical techniques, such as differential pulse voltammetry (DPV), cyclic voltammetry (CV), chronoamperometry, and coulometry were employed to clarify the mechanism of the electrode process. The compounds I and II with thiol group exhibited similar redox behavior. Both displayed two cathodic peaks, whereas the third compound, III, without thiol group showed only one cathodic peak in the same potential range of the second peak of I and II. The results of this study suggest that in the first step the one electron reduction of thiol produced a disulfide derivative and in the second reduction step the azomethane in the triazine ring was reduced in two electron processes. A reduction mechanism for all three compounds is proposed on this basis. In addition, some numerical constants, such as diffusion constant, transfer coefficient, and rate constant of coupled chemical reaction in the first reduction peak were also reported.

Evaluation of Design of Experiments to Develop MOF-5 Adsorbent for Acetylene Capture

  • Min Hyung Lee;Sangmin Lee;Kye Sang Yoo
    • Korean Chemical Engineering Research
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    • v.61 no.2
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    • pp.322-327
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    • 2023
  • A design of experiments was evaluated in optimizing MOF-5 synthesis for acetylene adsorption. At first, mixture design was used to optimize precursor concentration, terephthalic acid, zinc acetate dihydrate and N,N-dimethylformamide. More specifically, 13 conditions with various molar ratios were designed by extreme vertices design method. After preparing the samples, XRD, N2 physisorption and SEM analysis were performed for their characterization. Moreover, acetylene adsorption experiments were carried out over the samples under identical conditions. The optimal precursor composition for MOF-5 synthesis was predicted on a molar basis as follows: terephthalic acid : acetate dihydrate : dimethylformamide = 0.1 : 0.4 : 0.5. Thereafter, multi-level factorial design was designated to investigate the effect of synthesis reaction conditions such as temperature, time and stirring speed. By the statistical analysis of 18 samples designed, 4 reaction parameters were determined for additional adsorption experiments. Therefore, MOF-5 prepared under the synthesis time and temperature of 100 ℃ and 12 h, respectively, showed the maximum adsorption capacity of 15.1 mmol/g.

Synthesis of N,N-Dimethylacetamide from Carbonylation of Trimethylamine by Rhodium(I) Complex Under Anhydrous Condition

  • Hong, Jang-Hwan
    • Journal of Integrative Natural Science
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    • v.8 no.4
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    • pp.235-243
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    • 2015
  • Rhodium(I)-complex of $[Rh(CO)_2I_2{^-}]$ catalyzed carbonylation of anhydrous-trimethylamine in the presence of methyl iodide to give DMAC (N,N-dimethylacetamide) in no solvent. The catalyst had been reused 20 times, the analyses and distillation of collected products showed that the yields of DMAC, MAA (N-methylacetamide), and DMF (N,N-dimethylformamide) were 82.3%, 12.6%, and 4.4%. The conversion rate of trimethylamine was 99 % and the selectivity of DMAC was 82.3% with TON (Turnover Number) of 700. Stepwise procedure of inner-sphere reductive elimination for the formation of DMAC was suggested instead of acyl iodide intermediate.

Using Microwave Irradiation to Prepare New Poly(amide-imide)s Containing Tetrahydropyrimidinone, Tetrahydro-2-thioxopyrimidine, and Trimellitic Rings in Their Main Chains: Synthesis and Characterization

  • Faghihi Khalil;Hagibeygi Mohsen
    • Macromolecular Research
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    • v.13 no.1
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    • pp.14-18
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    • 2005
  • Under irradiation in a microwave oven, six novel poly(amide-imide)s containing tetrahydropyrimidinone, tetrahydro-2-thioxopyrimidine moieties and trimellitic rings in their main chains were synthesized through the polycondensation reaction of N,N'-(4,4'-diphenylether)bis(trimellitimide) diacid chloride with six different derivatives of tetrahydropyrimidinone and tetrahydro-2-thioxopyrimidine in the presence of a small amount of a polar organic medium, such as o-cresol. The polycondensation proceeded rapidly and completed within 7-9 min, producing a series of new poly(amide-imide)s in high yield that showed inherent viscosities in the range 0.33-0.52 dL/g. These poly(amide-imide)s were characterized by elemental analysis, viscosity measurement, thermal gravimetric analysis, solubility test, and FT-IR spectroscopy. All of the polymers were soluble at room temperature in polar solvents such as N,N-dimethylacetamide, N,N-dimethylformamide, dimethylsulfoxide, tetrahydrofuran, and N-methyl-2-pyrrolidone.

Preparation of Poly(imide-aramid-sulfone)s and their Thermal Properties (폴리(이미드-아라미드-설폰)의 합성과 그들의 열적성질)

  • Park, Hyung-Seok;Gong, Myoung-Seon
    • Polymer(Korea)
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    • v.36 no.4
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    • pp.427-433
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    • 2012
  • A series of poly(imide-aramid-sulfone)s with alternatingly introduced imide/aramid groups were prepared by reacting divinyl sulfone (DVS) and $N^1,N^4$-bis(4-(vinylsulfonyl)phenyl)terephthalamide (2) with pyromellitic diimide. Three model compounds, N-[2-(p-aminophnenylsulfonyl)ethyl]phthalimide (3), 2,2'-(2,2'-sulfonylbis(ethane-2,1-diyl))diisoindoline-1,3-dione (4), and N,N-bis(4-(2-(1,3-dioxoisoindolin-2-yl)ethylsulfonyl)phenyl)terephthalamide (5), resembling polymers were prepared with good yields by reacting p-aminophenyl vinyl sulfone, DVS, and 2 with phthalimide. Condensation polymerization was carried out by Michael-type addition reaction of the difunctional phthalimide group with the DVS group in the presence of tetrabutylammonium hydroxide (TBAH), resulting in poly(imide-aramid-sulfone)s 6-12 with moderate molecular weights and good yields. They were highly soluble in polar solvents such as N,N-dimethylformamide, dimethylsulfoxide, N-methylpyrrolidinone and tetrahydrofuran. The ratios of DVS/2 were 1/0, 3/1, 2/1, 1/1, 1/2, 1/3, and 0/1. Molecular weight and physical properties such as solubility, viscosity, and thermal properties of the polymers were examined.

Establishment of Analytical Method for Chlorophyll Using the N,N-Dimethylformamide and Dimethylsulfoxide in Citrus Leaves (N,N-Dimethylformamide와 Dimethylsulfoxide를 이용한 감귤 잎의 엽록소 측정방법 확립)

  • Han, Seung-Gab;Kang, Seok-Beom;Moon, Young-Il;Park, Jae-Ho;Park, Kyung-Jin;Choi, Young-Hun
    • Korean Journal of Environmental Agriculture
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    • v.33 no.4
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    • pp.344-349
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    • 2014
  • BACKGROUND: Purpose of the study was to establish the extinction coefficients of chlorophyll a and b in N,N-dimethylformamide(DMF) and Dimethylsulfoxide(DMSO) solvents and to find out the conditions of optimal extraction temperature and time in citrus leaves. METHODS AND RESULTS: Chlorophyll a and b standards were dissolved in DMF and DMSO. Extinction coefficients of chlorophyll pigments were determined and their contents were quantified using spectrophotometer. Chlorophyllous pigments of citrus(Citrus unshiu Marc. cv. Okitsu wase) leaves were extracted at 25, 40, 60 and $80^{\circ}C$ for 4, 6, 8, 24 and 48 hours to determine the optimal extraction condition. CONCLUSION: The extinction coefficients of chlorophyll a(Chl a) and chlorophyll b(Chl b) of DMF extracts for high extinction wavelength were 663.8 and 647.2 nm. Similarly, the high extinction wavelength of DMSO extracts were 665.8 and 649.0 nm for chl a and b respectively. Chl a, Chl b and total chlorophyll content of DMF extracts were Chl a = $12.10A_{663.8}-2.74A_{647.2}$, Chl b = $21.94A_{647.2}-5.06A_{663.8}$ and total $Chl=19.193A_{647.2}+7.04A_{663.8}$. Similarly, Chl a, Chl b and total Chl of DMSO extracts were Chl a = $14.53A_{665.8}-5.40A_{649.0}$, Chl b = $26.98A_{649.0}-7.11A_{665.8}$ and total $Chl=21.58A_{649.0}+7.43A_{665.8}$. The chlorophyll extracts of DMF and DMSO were very stable in dark. High chlorophyll contents of citrus leaves were found at $80^{\circ}C$ extraction for 6 hours in DMF and at $80^{\circ}C$ extraction for 24 hours in DMSO. However, the chlorophyll content was decreased significantly after 8 hours in DMF extraction while it was remained up to 30 hours in DMSO extraction.

A Study on the Insecticidal and Antibacterial Activity of the Carbamate derivatives (Carbamate 화합물의 殺蟲效果 및 抗菌力에 관한 연구)

  • Kang, Hoe-Yang;Jung, Chan
    • Journal of Environmental Health Sciences
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    • v.23 no.1
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    • pp.62-65
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    • 1997
  • The insecticidal and antibacterial activity of new synthesized carbamate derivatives(5,7-dibromo-8-hydroxyquinolinyl-N-methylcarbamate(I), 5,7-dibromo-8-hydroxyquinolinyl-N-ethylcarbamate(II)) was examined using 0.2w/v% acetone solutions and 50 $\mu$g/ml-1000 $\mu$g/ml N,N'-dimethylformamide H$_2$O(2:3) solutions of each compounds, respectively. 1. Two carbamates exerted insectiddal effects on Sogata furcifera HORVATH, Delphacodes Striatella FAUEN and Nilaparvate lugens STAL, Whereas no significant effects were observed on the Inazuma dorasalis MOISCHIULSKY Nephateffix apicalis Cincticeps UHLER. 2. These compounds exhibited growth-inhibitory activity against Staphyloccus aureus, Salmonella paratyphi A, Shigella dysenteriae 1a, Escherichia coli NL 1401, at the concentration range of 100-500 $\mu$g/ml in general.

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A Study on the Insecticidal and Antibacterial Activity of the 8-Hydroxy-5-chloroquinolyl Carbamates (8-Hydroxy-5-chloroquinolyl Carbamates의 살충효과 및 항균력에 관한 연구)

  • 강회양
    • Journal of Environmental Health Sciences
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    • v.21 no.1
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    • pp.74-77
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    • 1995
  • The insecticidal and antibacterial activity of new synthesized carbamate derivatives(8-Hydroxy-5-chloroquinolyl-N-methylcarbamate(I), 8-Hydroxy-5-chloroquinolyl-N-ethylcarbamate(II)) was examined using 0.2 w/v% acetone solutiolas and 50 r/ml~1000 r/m N,N'-dimethylformamide-$H_2O$(2:3) solutions of each compounds, respectively. 1) Two carbamates exerted insecticidal effects on Sogata furcifera HORVATH, Delphacodes Striatella FAUEN, Whereas no significant effects were observed on the Nilaparvate lugens STAL, Inazuma dorasails MOISCHIULSKY and Nephateffix apicalis Cincticeps UHLER. 2) These compounds exhibited growth-inhibitory activity against Staphylococcus aureus, Salmonella paratyphi A, Shigella dysenteriae 1a, Escherichia coli NL 1401,at the concentration range of 100~500 r/ml in general.

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