• Title/Summary/Keyword: high-pressure NMR

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Cosmetic Activities of Nyasol from the Rhizomes of Anemarrhena asphodeloide (지모의 뿌리줄기로부터 분리된 nyasol의 미용효과)

  • Park, Yhun Jung;Ku, Chang-Sub;Kim, Min-Jin;Lee, Mi Kyeong;Kim, Ki Ohk;Ryu, Hyung Won;Song, Hyuk-Hwan;Kim, Doo Young;Oh, Sei-Ryang
    • Journal of Applied Biological Chemistry
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    • v.58 no.1
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    • pp.31-38
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    • 2015
  • The rhizomes of Anemarrhena asphodeloide was extracted with 100% ethanol and concentrated subfractions were separated with medium pressure liquid chromatography-based activity profiling. One compound was isolated from the subfraction 10 through the repeated preparative high performance liquid chromatography (prep-HPLC). According to physico-chemical and spectroscopic data including NMR and MS, the chemical structures of the compound was determined as nyasol (1). Nyasol was exhibited potent inhibitory activity for NO ($IC_{50}:12.5{\mu}g/mL$), tyrosinase ($IC_{50}:12.5{\mu}g/mL$), melanin contents ($IC_{50}:12.5{\mu}g/mL$), thymus and activation-regulated chemokine (TARC) production ($IC_{50}:6.25{\mu}g/mL$). As a result, nyasol has an excellent inflammation-dependent anti-whitening and TARC production activity. It could be used to a large range of functional cosmetics.

Synthesis of polyphenylcarbosilane via thermal rearrangement of polymethylphenylsilane in supercritical cyclohexane

  • Shin, Hee-Yong;Ryu, Jae-Hun;Bae, Seong-Youl;Lee, Yoon-Joo;Kwon, Woo-Teck;Kim, Young-Hee;Kim, Soo-Ryong
    • Journal of the Korean Applied Science and Technology
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    • v.30 no.1
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    • pp.9-15
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    • 2013
  • A new process for the synthesis of polyphenylcarbosilane (PPCS) via thermal rearrangement of polymethylphenylsilane (PMPS) in supercritical cyclohexane was proposed and investigated at reaction temperatures of $380-420^{\circ}C$, reaction times of 1-2 h, and a pressure of 15 MPa. The structure, molecular weight, and molecular weight distribution of the product were characterized by FT-IR, Si-NMR, and GPC. The ceramic yield was also measured by TGA analysis. High-quality PPCS with high molecular weight and ceramic yield can be synthesized via a supercritical process. Furthermore, this process, when compared to the conventional method, tends to moderate the reaction conditions such as reaction temperature and time. It is concluded that thermal rearrangement in supercritical fluid is an efficient and viable process in terms of the resulting yield, efficiency, and reaction time compared with those of the conventional PCS production process.

The Study on the Synthesis of Triazole Derivatives as Energetic Plasticizer (트리아졸 계열의 에너지 가소제 합성 연구)

  • Lee, Woonghee;Kim, Minjun;Park, Youngchul
    • Journal of the Korean Society of Propulsion Engineers
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    • v.20 no.2
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    • pp.31-38
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    • 2016
  • Most of propellants that is used widely in the world release toxic gases such as methane gas and carbon dioxide during combustion which are noxious to the environment. This study established a synthetic process of a high nitrogen containing derivative of triazole, 4,5-bis(azidomethyl)-methyl-1,2,3-triazole (DAMTR), which can be applied as energetic plasticizer to environmental concerns. Also, the compound was characterized by NMR, IR spectroscopy, and physical properties such as glass transition temperature, melting point, decomposition temperature, density, impact sensitivity, viscosity and volatility were measured. In addition, the heats of formation (${\Delta}H_f$) and detonation properties (pressure and velocity) of DAMTR were calculated using Gaussian 09 and EXPLO5 programs.

Anti-inflammatory and Anti-oxidative Activities of Flavonoids Extracted from Dendranthema indicum Flowers in Jeju Island (제주 자생 감국 꽃 추출물 유래 flavonoid 화합물의 항산화 및 항염 활성)

  • Hyun, Ju Mi;Jo, Yeon Jeong;Kim, Yun Beom;Park, Sung-Min;Yoon, Kyung-Sup;Lee, Nam Ho
    • Journal of the Korean Applied Science and Technology
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    • v.36 no.4
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    • pp.1259-1267
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    • 2019
  • Anti-inflammatory and anti-oxidative activities were examined on the extract of Dendranthema indicum (D. indicum) flowers. The flowers were extracted two times for 24 h each with 70% ethanol. Upon the biological activities screening, the ethanol extract exhibited potent free radical scavenging activities and inhibited the production of nitric oxide on LPS-induced RAW264.7 macrophages effectively without causing cell toxicity. Further purification by medium pressure liquid hromatography (MPLC) and identification of the isolates led to identification of cynaroside (1) and apigetrin (2). The chemical structures of the isolated compounds were elucidated based on spectroscopic data including nuclear magnetic resonance (NMR) spectra, as well as comparison of the data to the literature values. Also, the quantitative analysis of the compounds was perfromed by high-performance liquid chromatography (HPLC). The isolates 1 and 2 were determined to inhibite the nitric oxide (NO) production dose-dependently. Based on these results, it was suggested that D. indicum extract could be useful as anti-inflammatory agents in cosmetics applications.

Identification of a Neolignan Glycoside from the Pine Tree, Pinus densiflora Showed Antithrombotic Activity (Pinus densiflora 유래의 항트롬빈 활성을 나타내는 Neolignan Glycoside의 동정)

  • Seo, Min-Jeong;Kang, Byoung-Won;Jeong, Yong-Kee
    • Journal of Life Science
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    • v.24 no.8
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    • pp.873-879
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    • 2014
  • The constituents from the needles of the pine tree, Pinus densiflora, were purified and investigated for antithrombotic activity. The needles were initially extracted three times with 70% ethanol, and the extract was sequentially fractionated with chloroform and n-butanol. The aqueous layer formed after n-butanol fractionation was subjected to purification by medium pressure and high pressure liquid chromatography. The two neolignans, 2, 3-dihydro-7-hydroxyl-3-hydroxymethyl-2-(4'-hydroxyl -3-methoxyphenyl)-5-benzofuranpropanol-3-O-${\alpha}$-rhamnopyranoside (a neolignan glycoside) and 2, 3-dihyro-3-hydroxymethyl-7-methoxy-2-(4'-hydroxyphenyl-3'-methoxy)-5-benxofuran propanol 4'-O-${\alpha}$-rhamnopyranoside (icariside $E_4$) were identified by $^1H$ and $^{13}C$ NMR spectra. The effect of the purified compounds, the neolignan glycoside and icariside $E_4$ on thrombin inhibition were investigated by measuring thrombin clotting time in plasma. As a result, the clotting of the neolignan glycoside was delayed four times compared to that of icariside $E_4$. In addition, an analysis of the inhibition effect by changing the concentration showed that the clotting time was delayed in accordance with an increase in the concentration of the neolignan glycoside. Furthermore, we examined the interaction of thrombin and fibrinogen to clarify the action mechanism. As a result, the delay of clotting time in the response of thrombin and pure fibrinogen may indicate that neolignan glycosides inhibit the thrombin action in a direct manner, leading to the suppression of fibrin generation.

Synthesis of Pressure-sensitive Acrylic Adhesives with Photoreactive Groups and Their Application to Semiconductor Dicing Tapes (광 반응성기를 갖는 아크릴 점착제의 합성과 반도체 다이싱 테이프로의 적용 연구)

  • Hee-Woong Park;Nam-Gyu Jang;Kiok Kwon;Seunghan Shin
    • Applied Chemistry for Engineering
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    • v.34 no.5
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    • pp.522-528
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    • 2023
  • In this work, adhesive tapes were prepared for the dicing process in semiconductor manufacturing. Compounds with different numbers of photoreactive groups (f = 1 to 3) were synthesized and incorporated into acrylic copolymers to formulate UV-curable acrylic adhesives. Structural confirmation of the synthesized photoreactive compounds (f = 2 or 3) was performed using nuclear magnetic resonance (NMR) spectroscopy. The introduction of the photoreactive compounds into the acrylic adhesive was accomplished by urethane reactions, and the successful synthesis of the UV-curable acrylic adhesive was verified by Fourier transform infrared (FT-IR) measurements. To evaluate the performance of the adhesive, the peel strength was evaluated before and after UV irradiation using a silicon wafer as a substrate. The adhesive exhibited high peel strength (~2000 gf/25 mm) before UV exposure, which was significantly reduced (~5 gf/25 mm) after UV exposure. Interestingly, the adhesive containing multifunctional photoreactive compounds showed the most significant reduction in peel strength. In addition, surface residue measurements by field emission scanning electron microscopy (FE-SEM) showed minimal surface residue (~0.2%) after UV exposure. Overall, these results contribute to the understanding of the behavior of UV-curable acrylic adhesives and pave the way for potential applications in semiconductor manufacturing processes.

Synthesis and Properties of Glucamine Derivatives with New Composition (새로운 조성을 갖는 글루카민 유도체의 합성 및 계면성)

  • Park, Seon-Young;Kim, Tae-Young;Jeong, Hwan-Kyeong;Nam, Ki-Dae
    • Journal of the Korean Applied Science and Technology
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    • v.17 no.3
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    • pp.149-157
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    • 2000
  • The synthesis of N-methyl glucamine was performed in two step reaction. The first step involves the amination between methylamine and glucose in methane. The N-methyl glucamine was obtained by the reduction of using Ni catalyst under the high pressure. The second step was glucamide anionic derivatives synthesis from N-methyl glucamine, maleic anhydride, lauryl alcohol and laurylamine by Schotten Banmann reaction respectively. Their molecular structures of N-methyl glucamine and glucamide (EG-MAS and AC-MAS) were investigated by IR and $^{1}H-NMR$. Basic physical properties and biodegradability of there glucamide anionic surfactant was investigated. The range of cmc values determined by measurements of surface tention was $10^{-5}{\sim}10^{-4}mol/l$ and the surface tension of the aqueous solution revealed in the range $28{\sim}30$ dyne/cm and their biodegradability was very good in the pH $5{\sim}10$.

Synthesis of Nonionic Sorbitan Monostearate Using High Purity 1,4-sorbitan (고순도 1,4-솔비탄을 이용한 비이온 솔비탄 모노스테아르산 합성)

  • Yu, Hwa-Yeal;Ju, Chang-Sik;Moon, Bu-Hyun;Kim, Young-Seok;Lee, Ju-Dong;Lee, Man-Sig
    • Journal of the Korean institute of surface engineering
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    • v.41 no.2
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    • pp.51-56
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    • 2008
  • Nonionic sorbitan monostearate have been successfully prepared by esterification using 1,4-sorbitan and stearic acid. 1,4-sorbitan were prepared using D-sorbitol and acid catalyst at solvent-free conditions. The synthesized surfactants were characterized by NMR and FT-IR. We also investigated the effect of temperature, pressure and catalyst on the synthesis of nonionic sorbitan monostearate. The yields of 1,4-sorbitan were 90% at $160^{\circ}C$ under 160 mmHg vacuum, and the yields of nonionic sorbitan monostearate were 92% at $230^{\circ}C$ under 60 mmHg vacuum.

Purification of Antifungal Antibiotic NH-B1 from Actinomycete NH 50 Antagonistic to Plant Pathogenic Fungi (식물병원진균에 길항효과가 있는 방선균 균주 NH50에서 항진균성 항생물질 NH-B1의 순수 분리)

  • 김현겸;김범석;문석식;황병국
    • Korean Journal Plant Pathology
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    • v.14 no.3
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    • pp.191-202
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    • 1998
  • About 300 actinomycetes were isolated from two forest and one sea-shore soil and tested for inhibitory effects on mycelial growth of six plant pathogenic fungi Magnaporthe grisea, Alternaria mali, Colletotrichum gloeosporioides, Phytophthora capsici, Fusarium oxysporum f. sp. cucumerinum, and Rhizoctonia solani. Among 300 actinomycetes tested, only 16 actinomycetes showed the antifungal activity against the test fungi. Isolate NH 50 was selected for production and purification of antifungal antibiotic substances. Actinomycete isolate NH 50 displayed the broad antifungal spectra against 11 plant pathogenic fungi. To identify actinomycete isolate NH 50, cultural characteristics on various agar media, diaminopimelic acid type, and morphological characteristics by scanning electron microscopy were examined. As a result, actinomycete isolate NH 50 was classified as a rare actinomycete that had LL-DAP type and did not produce spores. After incubation of isolate NH 50 in yeast extract-malt extract-dextrose broth, antifungal compound NH-B1 that inhibited mycelial growth of some plant pathogenic fungi was purified from the methanol eluates of XAD-16 resins by a series of purification procedures, i.e., silica gel flash chromatography, C18 flash chromatography, Sephadex LH-20 column chromatography, silica gel medium pressure liquid chromatography (MPLC), C18 MPLC, and high pressure liquid chromatography (HPLC). UV spectrum and 1HNMR spectrum of antifungal compound NH-B1 dissolved in methanol were examined. The antibiotic NH-B1 showed the major peaks at 230 and 271.2nm. Based on the data of 1H-NMR spectrum, NH-B1 was confirmed to be an extremely complex polymer of sugars called polysaccharides. The antibiotic NH-B1 showed strong antifungal activity against Alternaria solani and Cercospora kikuchi, but weak activity against M. grisea.

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Study on Chemical Stabilities with R-1234yf Refrigerant of Polyol Ester Refrigerant Oil for Electric Vehicles (전기 자동차용 폴리올 에스테르계 냉동기유의 R-1234yf 냉매와의 적합성 연구)

  • Hong, J.S.;Chung, K.W.;Kim, N.K.;Shin, J.H.;Kim, Young Woon;Lee, E.H.;Go, B.S.;Hwang, S.Y.
    • Tribology and Lubricants
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    • v.36 no.3
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    • pp.139-146
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    • 2020
  • Global warming has led to an increase in demand of eco-friendly vehicles, such as electric cars, for reducing greenhouse gas emissions, and especially, regulating carbon dioxide generation. In addition, electric vehicles are equipped with an electric drive-type hermetic scroll compressor and a refrigerant, which exhibit current and future trends of using environmentally friendly refrigerants, including R-1234yf. In this study, polyol ester-based refrigeration oils are prepared via condensation esterification of polyol and fatty acids. The oils can be combined with R-1234yf refrigerant for applications in air conditioning and cooling systems of electric vehicles. The structure of synthetic polyol esters is confirmed via 1H-NMR and FT-IR spectrum analysis, and the composition of the polyol ester is analyzed via gas chromatogram analysis. Furthermore, kinematic viscosity, viscosity index, total acid value, pour point, and color are analyzed as fundamental physical properties of the synthetic polyol esters. The compatibility and chemical stability of the synthetic polyol ester combined with the R-1234yf refrigerant are obtained via high temperature and high pressure oil-resistant refrigerant tests. The changes in the oil color and catalyst activity are observed before and after the experiment to determine whether it is suitable as a refrigerator oil.