• Title/Summary/Keyword: Sulfonyl chloride

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Properties and Controls of hazardous gases from Electrochemical fluorination of Methanesulfonyl chloride (Methanesulfonyl Chloride의 전해불소화 반응 중 유해가스의 생성 및 제어)

  • 태범석;이종일;박영우
    • Journal of the Korean Society of Safety
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    • v.11 no.3
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    • pp.126-136
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    • 1996
  • Synthesis of perfluoromethanesulfonyl fluoride(PFMSF) which is a valuable precursor of perfluoro-chemicals such as surface modifier and fine chemicals was studied by electrochemical fluorination (ECF). In order to determine the termination of preelectrolysis, it was carried to monitor the variation of current during preelectrolysis by means of constant cell voltage operation. In a batch cell, chronopotentiometric electrolysis and various chemical analysis such as GC, GC/MS and If were used to understand the potential change of electrode and synthesis and control of hazardous gases products. Termination of preelectrolysis was determinated by measurement the current and/or detection of $F_2$ gas generation. And during the preelectrolysis, an amount of generated $OF_2$ was shown that a lot of moisture was absorbed from air when a cell was filled with anhydrous hydrogen fluoride( AHF ). Above 4V cell voltage, $F_2$ gas was generated and acted on any form of fluorinating agents. In the ECF of MSC (methane sulfonyl chloride) by constant current operation, the potential of anode was intimately relation with generation of $SO_2F_2$. Exchange of Cl to F was dominatly occured in a initial stage. There were various gaseous products including PFMSF as main product and $C_4$ compounds.

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Studies on 1,2-Naphthoquinone-(2)diazide-5-sulfonic Acid Ester Derivatives for Pre-sensitized Offset Plates (PS 판용 1,2-Naphthoquinone-(2)diazide-5-sulfonic Acid Ester Derivatives의 합성 및 응용)

  • Ku, Yang Seo;Myung, Young Chan;Ahn, Chong Il;Kim, Sun Ho
    • Applied Chemistry for Engineering
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    • v.10 no.8
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    • pp.1169-1174
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    • 1999
  • 2-Diazo-1-naphthoquinone-5-sulfonyl chloride(NQD-Cl) was synthesized from sodium 2-diazo-naphthoquinone-5-sulfonate by chlorination. NQD-Cl was esterified with hydroxybenzophenones to give several 1,2-naphthoquinone-(2)-diazide-5-sulfonic acid ester derivatives(NQD-esters). We have compared benzophenone derivatives with methoxy group to benzophenone derivatives with hydroxy group. Solubility of each NQD-ester was studied. Each of NQD-esters was formulated with novolac base resin and PS plates were manufactured. Photosensitivity, bleachability, compatible exposed time and relative sensitivity were determined by UV spectrophotometry, imaged by UV lithographic techniques, and the gray scale method. According to the number of substituted NQD group, it showed that relative sensitivity was different from gray scale method. NQD-esters with methoxy group showed a good solubility and higher sensitivity than commercial PS ones.

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Determination of Free 4-hydroxyproline with Dansylchloride by HPLC in Human Urine (소변 중 4-hydroxyproline 분석에 관한 연구)

  • Lee, Keou-Weon;Cho, Young-Bong;Lee, Kyung-Jong
    • Journal of Preventive Medicine and Public Health
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    • v.35 no.4
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    • pp.282-286
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    • 2002
  • Objectives : The level of 4-hydroxyproline (4-Hyp) in human urine was measured using high performance liquid chromatography (HPLC) with a fluorescence detector. This method is useful for medical examinations and investigating the radicals induced by physical, chemical, mental stresses. This method is superior to many published several methods in terms of its low cost and ability to analyze many samples. Methods : The urine from workers in a tire manufacturing company (22 male pre- and post-shift workers) and 18 office-workers as controls were analyzed. Data concerning age, the cumulative drinking amount and the cumulative smoking amount was collected with a questionnaire. The optimum applied amount of dansyl-Cl, the optimum reaction temperature and time, the recoveries and the optimum pH of the eluent and buffer were determined.4-Hyp from human urine was derivatized with dansyl-Cl (dimethylamino-naphthalene-1-sulfonyl chloride) after removing the a-amino acid by a treatment with phthalic dicarboxaldehyde (OPA) and cleaned with Bond Elut C18 column. The 4-Hyp derivatives were separated on a reversed phase column by gradient elution with a phosphate buffer (5 mmol, pH 8.0) and acetonitrile, and detected by fluorescence measurements at 340 nm (excitation) and 538 nm (emission). Results : The detection limit for the urinary free 4-Hyp was $0.364{\mu}mol/l$. The recovery rate of 4-Hyp was 99.7%, and the effective pH of the phosphate buffer and borate buffer were 3.0 and 8.0, respectively. From statistical analysis, age, drinking and smoking did not affect the urinary free 4-Hyp in both the controls and workers. The range of urinary 4-Hyp in the controls, pre-shift, and post-shift workers were 0.33-16.44, N.D-49.06, and $0.32-56.27{\mu}mol/l$. From the pared-sample t-test, the urinary 4-Hyp levels in post-shift workers ($11.82{\pm}6.73\;nmmol/mg\;Cre$) were 2-fold higher than in pre-shift workers ($5.36{\pm}5.53\;nmol;/mg\;Cre$) and controls ($4.91{\pm}4.89\;nmol;/mg\;Cre$). Conclusions : This method was developed with high sensitivity, accuracy, and precision. The present method was effectively applied to analyze the urinary free 4-Hyp in both controls and workers.

Cell-Specific Targeting of Texas Red with Anti-Ep-CAM Antibody

  • Lee, Soo-Chul;Tae, Gun-Sik
    • Journal of Photoscience
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    • v.12 no.3
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    • pp.123-127
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    • 2005
  • The polyclonal antibody was generated against the peptide fragment of 62 amino acid residues (D 181-T242) near the COOH-terminal region of the extracellular domain of epithelial-cell adhesion molecule (Ep-CAM) and shown to be able to recognize Ep-CAM in competitive ELISA. Then, sulforhodamine 101 acid chloride (so called Texas red), a fluorescence dye, was conjugated to the affinity-purified anti-Ep-CAM antibody utilizing the reaction between the aliphatic amines of antibody and the sulfonyl chloride of Texas red. The molar ratio of Texas red to antibody was estimated to be approximately 1.86 by measuring optical densities at 280 nm and 596 nm, implying that the two molecules of Texas red at most were conjugated to antibody. The anti-Ep-CAM antibody-Texas red conjugate was then used for immunohistochemistry of CT-26 murine colon carcinoma cells. Based upon the fluorescence microscope images, anti-Ep-CAM antibody is able to deliver Texas red specifically to the surface of CT-26 cells on which Ep-CAM was actively expressed. This result indicates that anti-Ep-CAM antibody could be useful for the tissue-specific delivery of photosensitizers via antigen-antibody interaction.

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A Study on the Preparation and Properties of Chlorosulfonated Polyethylene Modified Polyvinylchoride (Chlorosulfonated Polyethylene으로 개질된 Polyvinylchloride의 제조와 물성)

  • Ahn, Jae-Joon;Lee, Seung-Tae;Kim, Byung-Kyu;Shin, Young-Jo
    • Applied Chemistry for Engineering
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    • v.5 no.2
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    • pp.215-222
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    • 1994
  • As a toughness modifier for plastics chlorosulfonated polyethylene(CSM) can be used. CSM has a good resistance to oxygen and ozone. CSM has a crosslinkable functional group(sulfonyl chorid) with sulfur and metal oxide. Polyvinylchloride(PVC) is widely used industrial plastics because of its balanced properties and low cost. But it has some disadvantages such as low impact strength, light, ozone and oxygen degradation. In order to improve these properties of PVC, CSM was blended with PVC. The toughening effect appeared at about 10wt% and there is no additional effect above 30wt% of CSM. The weatherability, ozone resistance and mechanical properties of PVC were improved by blending with CSM. The toughening mechanism is studied by SEM.

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Reverse-Phase High Performance Liquid Chromatographic Determination of Amino Acids after Precolumn Derivatization with 1-Dimethyl-aminonaphthalene-5-sulfonyl chloride (Dansyl 유도체화와 역상 고성능액체크로마토그래피에 의한 아미노산의 정량)

  • 나혜경;전덕영;홍윤호
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.22 no.6
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    • pp.815-822
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    • 1993
  • This experiment was carried out to determine the separation condition of 1-dimethylaminonaphthalene-5-sulfony(Dansyl) derivatives of amino acids by reverse-phase high performance liquid chromatography with Nova-Pak C18 column. Determined solvent system was solvent A(200mA phosphate buffer pH 6.8 15%, acetonitrile 11%, water 74%) and solvent B(acetonitrile 65%, methanol 28%, water 7%). Linear gradient of solvent B was applied from 12% to 80% for 50min. Complete separation of 20 amino acids including asparagine and glutamine which constitute protein was achieved within 50min. As the detection limit was the range of picomole, the resolution power was excellent. Reproducibility of the retention time was less than mean $\pm$0.05min. According to the above optimum chromatographic conditions, the amino acid composition of some food and human blood was examined. The most affluent amino acid was alanine in human blood, aspartic acid and glutamic acid in soy sauce, alanine and threonine in soy milk and proline in milk and yoghurt.

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Photosensitive Polyimides Having Aromatic Sulfonyloxyimide Groups in the Main Chain (주쇄에 광분해성 방향족 술포닐옥시이미드기를 함유한 감광성 폴리이미드)

  • 오세용;이지영;조성열;정찬문
    • Polymer(Korea)
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    • v.24 no.3
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    • pp.407-417
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    • 2000
  • Photosensitive polyimides having cyclobutane or phenyl and aromatic sulfonyloxyimide units in the main chain have been synthesized and the photodegradation behavior was investigated in relation with the polymer structure. The polyimides were prepared by condensation polymerization of N-hydroxyl and sulfonyl chloride. The prepared polyimides were stable up to 25$0^{\circ}C$ without thermal degradation. It has been found that the photodegradation of polyimides upon irradiation of 254 nm UV light results from scission of N-O bonds or ring opening of imides moiety by spectroscopic measurements. The polyimides were useful as positive working photodegradable polymers. Especially, the positive tone image of polyimide containing a pyromellitic diimide moiety exhibited high sensitivity and resolution.

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Morecular Orbital Caculations for the Reactions of 2,5-dimethyl Pyrrole with Phenylsulfonyl Chloride

  • 서미경;김진범;성시열;심영기
    • Bulletin of the Korean Chemical Society
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    • v.20 no.8
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    • pp.948-952
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    • 1999
  • Electrophilic substitutions on β-position of 2,5-dimethyl pyrrole have been investigated theoretically. The electron donating methyl groups enrich electron densities on C-3, C-4 positions and π* interactions with methyl groups substituted on C-2 and C-5 positions pushed up the HOMO level of the pyrroles consequently induce rapid substitutions on C-3, C-4 sites. Substitution of phenylsulfonyl group on nitrogen stabilized LUMO levels through weak π bonding interactions. Unexpected deoxidation reaction underwent on the sulfonyl group substituted at C-3 position. The structures were solved by X-ray crystallography. Meanwhile, gas phase HF/6-31G* and density functional method (B3LYP/6-31G*) calculations gave favorable energies for 1-phenylsulfinyl pyrrole (6) over 3-phenylsulfinyl pyrrole (5) by 3.6-4.7 kcal/mol which is contrary to the experimental result. However the methods involve the effects of molecular polarizability and solvent, molecular dynamics (MD) and ab-initio self consistent reaction field (SCRF) calculations showed same trend as experiments. According to MD calculations, compound 5 is more stable than compound 6 by 4.15 kcal/mol and the SCRF, HF/6-31G* calculations gave more stable energy value for structure 5 than 6 by 0.03 kcal/mol.

Photochemistry of o-Nitrobenzyl System Coupled with a Benzylsulfonyl Chromophore (벤질술포닐 흡광단에 결합된 2-니트로벤질계의 광화학에 관한 연구)

  • Kim, Hee Jong;Chang, Sun Ki;Choo, Dong Joon
    • Applied Chemistry for Engineering
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    • v.10 no.1
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    • pp.124-128
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    • 1999
  • The photochemistry of the derivatives of o-nitrobenzylcarboxyl esters or benzylsulfonyl derivatives has been well studied separately. But little attempt has been made to combine the fruits these two studies. Being photochemically active, benzylsulphonyl and intro groups should influence the reactivity of each other's, especially when the excited states are fully mixed due to the proximity of their location. The questions which should be clearly answered are; what kind of effect will be excerted to the other group, and whether these two functional groups are coupled in the course of the reaction. To answer the questions raised above, wer have synthesized two sulfonyl esters and four amides from the newly available starting material, 2-nitro-${\alpha}$-toluenesulfonyl chloride. The products identified from the exploratory solution photochemistry were cyclohexanol, phenol, cyclohexylamine, and sulfur dioxide. The results are not much different from the products originally anticipated. It has been temporarily concluded that there is little interaction between the benzyl sulfonyl group and ortho-nitro chromophore. The fact that a base (an amine) has been photochemically generated in solution photochemistry was further confirmed by and utilized in the solid phase quantitative photochemistry done on the film, so as to carry out the photochemical epoxide cure.

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Effects of Taurine Supplementation on Serum Lipidperoxide Levels in Middle-aged Women (중년 여성에 있어 타우린 보충 급여가 혈청 지질 과산화물 농도에 미치는 영향)

  • Ahn, Chang-Soon
    • The Korean Journal of Food And Nutrition
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    • v.20 no.4
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    • pp.440-449
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    • 2007
  • The purpose of this study was to examine the effects of taurine supplementation on serum lipidperoxide(TBARS), a risk factor for cardiovascular disease. The subjects were 22 healthy middle-aged women(33 to 54 years). Serum lipids, thiobarbituric acid reactive substances(TBARS), and plasma taurine levels were measured before and after supplying 3 g of taurine per day for 4 weeks. Plasma taurine was analyzed by Dabsyl-Cl(4-dimethylamino azobenzen-4-sulfonyl-chloride) derivatization and reversed-phase HPLC. Serum TBARS was measured by the Yagi method. Daily dietary taurine intake was calculated by food frequency questionnaire method. The weight and height means of the 22 subjects were $57.9{\pm}5.2$ kg and $159.2{\pm}5.2$ cm, respectively. Their percent body fat and waist/hip ratio(WHR) were 26.8% and 0.84, respectively, which were slightly higher than the average for middle-aged Korean women. Serum TC, TG and LDL-C levels tended to decrease after taurine supplementation, but HDL-C was not changed. A positive correlation between plasma taurine and HDL-C was shown after taurine supplementation. The serum TBARS concentration was significantly decreased from $5.05{\pm}0.84nmol/d{\ell}$ to $4.17{\pm}0.64nmol/d{\ell}$ after taking taurine(p<0.01), and the plasma taurine concentration was significantly increased from $63.7{\pm}14.2{\mu}mol/{\ell}$ to $73.8{\pm}16.6{\mu}mol/{\ell}$ after taurine supplementation(p<0.05). The average dietary intake of taurine was $178.5{\pm}50.4$ mg/day, which is similar to the average daily taurine intake of Korean women. In conclusion, taurine is an effective nutrient that antagonizes TBARS levels. Therefore, this study suggests that a sufficient taurine intake may be an effective way to prevent cardiovascular disease such as atherosclerosis.