• 제목/요약/키워드: Selective hydrolysis

검색결과 66건 처리시간 0.03초

Synthesis and Characterization of Various Di-N-Functionalized Tetraaza Macrocyclic Copper(II) Complexes

  • Kang, Shin-Geol;Kim, Na-Hee;Lee, Rae-Eun;Jeong, Jong-Hwa
    • Bulletin of the Korean Chemical Society
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    • 제28권10호
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    • pp.1781-1786
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    • 2007
  • Two copper(II) complexes, [CuL3](ClO4)2 bearing one N-CH2CH2CONH2 group as well as one N-CH2CH2CN group and [CuL4](ClO4)2 bearing two N-CH2CH2CONH2 groups, have been prepared by the selective hydrolysis of [CuL2](ClO4)2 (L2 = C-meso-1,8-bis(cyanoethyl)-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane). The complex [CuL5](ClO4)2 bearing one N-CH2CH2C(=NH)OCH3 and one N-CH2CH2CN groups has been prepared as the major product from the reaction of [CuL2](ClO4)2 with methanol in the presence of triethylamine. In acidic aqueous solution, the N-CH2CH2C(=NH)OCH3 group of [CuL5](ClO4)2 undergoes hydrolysis to yield [CuL6](ClO4)2 bearing both N-CH2CH2COOCH3 and N-CH2CH2CN groups. The crystal structure of [CuL5](ClO4)2 shows that the complex has a slightly distorted square-pyramidal coordination polyhedron with an apical Cu-N (N-CH2CH2C(=NH)OCH3 group) bond. The apical Cu-N bond distance (2.269(3) A) is ca. 0.06 A longer than the apical Cu-O (N-CH2CH2CONH2 group) bond of [CuL4](ClO4)2. The pendant amide group of [CuL3](ClO4)2 is involved in coordination. The carboxylic ester group of [CuL6](ClO4)2 is also coordinated to the metal ion in various solvents but is removed from the coordination sphere in the solid state.

Isotope-Dilution Mass Spectrometry for Quantification of Urinary Active Androgens Separated by Gas Chromatography

  • Lee, Su-Hyeon;Choi, Man-Ho;Lee, Won-Yong;Chung, Bong-Chul
    • Mass Spectrometry Letters
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    • 제1권1호
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    • pp.29-32
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    • 2010
  • Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methods are needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry (GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which are clinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with $\beta$-glucuronidase, solid-phase extraction, liquid-liquid extraction using methyl tert-butyl ether and subsequent conversion to pentafluorophenyldimethylsilyl-trimethylsilyl (flophemesyl-TMS) derivatives for sensitive and selective analysis in selected-ion monitoring mode. Flophemesyl-TMS derivatization not only eliminates matrix interference but also has a good peak resolution within a 6 min-run. A selective and sensitive GC technique with flophemesyl-TMS derivatives also allows accurate quantitative analysis of three active androgens when combined with IDMS. The limit of quantification of the three analytes was <50 pg/mL, and extraction recoveries ranged from 91.9 to 102.1%. The precision and accuracy were 1.2~6.5% and 89.0~106.7%, respectively. This GC-IDMS method can be useful for evaluating the drug efficacy and monitoring the biological processes responsible for male-pattern baldness and prostate diseases.

Preparation of an Amino Acid Based DTPA as a BFCA for Radioimmunotherapy

  • Choi, Kang-hyuk;Hong, Young-Don;Pyun, Mi-Sun;Choi, Sun-Ju
    • Bulletin of the Korean Chemical Society
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    • 제27권8호
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    • pp.1194-1198
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    • 2006
  • For the purpose of developing more effective chelating agents, we have synthesized a diethylene triamine pentaacetic acid(DTPA) analogue by using an amino acid. S-(N-Boc-aminophenyl)-Cys(t-Bu4-DTPA) methylester was prepared in 6 steps with total yield of 47.9%. For the sake of introducing a biomolecule to the DTPA derivative, a selective hydrolysis was performed with 3 M HCl/Ethylacetate = 1 : 3 ($25{^{\circ}C}$, 30 min, vigorous stirring). $^{166}Ho$-Cys-DTPA and $^{166}Ho$-Biotin-Cys-DTPA were prepared by mixing $^{166}Ho$ with DTPA derivatives at room temp in a HCl solution (pH = 5) and the radiochemical stabilities (> 99%) were maintained for over 6 hrs in vitro.

Characterization of Pyribenzoxim Metabolizing Enzymes in Rat Liver Microsomes

  • Liu Kwang-Hyeon;Moon Joon-Kwan;Seo Jong-Su;Park Byeoung-Soo;Koo Suk-Jin;Lee Hye-Suk;Kim Jeong-Han
    • Toxicological Research
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    • 제22권1호
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    • pp.1-8
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    • 2006
  • The primary metabolism of pyribenzoxim was studied in rat liver microsomes in order to identify the cytochrome P450 (CYP) isoform(s) and esterases involved in the metabolism of pyribenzoxim. Chemical inhibition using CYP isoform-selective inhibitors such as ${\alpha}$-naphthoflavone, tolbutamide, quinine, chlorzoxazone, troleandomycin, and undecynoic acid indicated that CYP1A and CYP2D are responsible for the oxidative metabolism of pyribenzoxim. And inhibitory studies using eserine, bis-nitrophenol phosphate, dibucaine, and mercuric chloride indicated pyribenzoxim hydrolysis involved in microsomal carboxylesterases containing an SH group (cysteine) at the active center.

잎담배중 유리 및 Glycoside형태로 존재하는 휘발성 향기성분 (Free and Glycosidically Bound Volatile Components in Tobacco Leaves(Nicotiana tabacum L.))

  • 김영회;나도영;김옥찬;서철원;김용태
    • 한국연초학회지
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    • 제14권1호
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    • pp.79-86
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    • 1992
  • Free and glycosidically bound volatiles from three green tobacco leaves(NC 82, KF 109 and Br-21) were separated by nonionic resin Amberlite XAD-2 adsorption column chromatography and election by selective solvents. Aglycones from the glycosidically bound fractions were released by enzymatic hydrolysis with almond B-glucosidase. A total of 20 components identified from free and glycosidically bound fractions, the major components were benzaldehyde, benzyl alcohol, 2-phenylethyl alcohol, 3-oxo- -ionol, 3-hydroxy-B-ionone, 3-oxo-7, 8-dihydro-n-ionol and scopoletin. Six Cl.B norisoprenoids identified in this study, which have been described to possess a characteristic tobacco aroma-enhancing effect, were not presented in free forms but rather bound glycosidic forms.

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Synthesis of Amphiphilic Poly(alkyl methacrylate-b-methacrylic acid) by Group Transfer Polymerization and Selective Hydrolysis

  • Soon Ki Kwon;Weon Jung Choi;Yun Hi Kim;Sam Kwon Choi
    • Bulletin of the Korean Chemical Society
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    • 제13권5호
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    • pp.479-482
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    • 1992
  • Several poly(alkyl methacrylate-b-t-butyl methacrylate) diblock copolymers were synthesized by group transfer polymerization. The molecular weight of poly(t-butyl methacrylate) segments and the composition of the resulting block copolymers were controlled by the monomer feed ratios and mole ratios of monomer to initiator. The poly(t-butyl methacrylate) block was quantitatively hydrolyzed to poly(methacrylic acid) block by refluxing with a catalytic amount of p-toluenesulfonic acid in dioxane at $100^{\circ}C$ for 12 hrs. The thermogravimetric analysis of poly(alkyl methacrylate-b-t-butyl methacrylate) exhibited the lose of isobutylene and subsequent anhydride formation in the range of $205-300^{\circ}C$.

키틴과 키토산 분해 미생물 유래 효소의 식품에의 이용 (Food application of enzymes derived from microorganisms degrading chitin and chitosan)

  • 박제권
    • 식품과학과 산업
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    • 제53권1호
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    • pp.43-55
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    • 2020
  • Most reports demonstrated the substrate specificity-based kinetic properties of chitin or chitosan degrading enzymes. However, there is virtually less information on the high quality and quantity production of chitin or chitosan hydrolysates having a larger than (GlcN)7 from the hydrolysis of high molecular weight chitosan using specific enzymes and their biological activity. Therefore, the production of such molecules and the discovery of such enzyme sources are very important. Fortunately, the author has established a mass production method of chitosan hydrolysates (GlcN)n, n=2-13 that have been characterized as a potent antioxidant substance, as well as antifungal and antibacterial activities against Penicillium species and highly selective pathogenic bacteria. In addition, preclinical studies using (GlcN)n, n=5-25 demonstrated that these molecules played a very important role in maintaining biometric balance. Collectively, it is implicated that the application of these mixed substances to foods with significant biological activity is very encouraging.

An Asymmetric Synthesis of (+)-Polyoxamic acid

  • Lee, Ki-Han;Oh, Chang-Young;Lee, Kee-Young;Kim, Yong-Hyun;Lee, Yiu-Suk;Joo, Jae-Eun;Ham, Won-Hun
    • 대한약학회:학술대회논문집
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    • 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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    • pp.362.3-362.3
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    • 2002
  • The Polyoxin complex is an antifungal antibiotics produced by Streptomyces cacaoi var. asoensis that exhibit marked and selective activity against pytopathogenic fungi. They incorporate carbamoylated dipeptides attached to the sugar moiety. Controlled alkaline hydrolysis of polyoxins result in several products. one of which has been identified as (+)-(2S. 3S, 4S)-2-amino-3. 4. 5-trihydroxypentonic acid(polyoxamic acid). A variety of chemical syntheses of polyoxamic acid have been developed over several years. (omitted)

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유효충돌빈도를 고려한 암모니아 생성 증대기법 연구 (Study on Enhancement of Ammonia Generation for Effective Collision Frequency)

  • 김세진;최용석;박현철
    • 항공우주시스템공학회지
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    • 제17권6호
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    • pp.1-8
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    • 2023
  • 기후변화 대응을 위하여, 항공 분야를 포함한 운송 분야에서 국제온실가스 감축제도 도입 추진 및 대체 에너지 개발 등 환경문제에 대한 연구개발이 활발하다. 그 중 무탄소 에너지원으로 주목받는 암모니아 연료에 대한 관심이 증대되고 있다. 암모니아는 액화 및 운반이 용이하며, 메탄올과 비슷한 에너지 밀도 등의 장점이 있다. 그러나 폭발성 및 독성으로 취급성이 어렵다. 본 연구에서는 암모니아에 비해 취급이 용이한 요소수에 고온의 수분으로 열분해와 가수분해 반응을 유도하여 안정적인 암모니아 발생을 시도하고자 하였다. 암모니아 가수분해 촉진을 위해 고온의 증기를 이용하였고 이론 당량비 미만의 암모니아 발생원인 규명을 하고자 했다. 기체분자운동론에 기인하여 가수분해 촉진을 위한 충분한 충돌빈도가 이루어지지 않았다는 가설을 수립했다. 수분 공급량 변화를 통해 미반응 이소시안산의 가수분해 여부를 실험하였고 암모니아 발생량이 증가함을 확인하였다. 일정 구간동안 암모니아 발생량 증가는 증기 온도, 수분공급유량에 종속됨을 알 수 있었다.

표면음향파 화학센서를 이용한 수용액 중 시안화이온의 선택적인 고감도 검출 (Highly sensitive and selective detection of cyanide in aqueous solutions using a surface acoustic wave chemical sensor)

  • 이수석
    • 한국음향학회지
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    • 제35권6호
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    • pp.473-479
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    • 2016
  • 본 연구는 센서 표면에 고정된 티오에스터 분자와 금 나노입자를 이용하여 수용액 중의 시안화이온(cyanide)을 선택적이고, 고민감도로 검출할 수 있는 200 MHz 표면음향파(Surface Acoustic Wave, SAW) 센서의 개발에 관한 것이다. SAW 센서표면에 형성된 티오에스터 단분자막은 시안화이온의 친핵성 첨가반응에 의해 가수분해되어 티올(thiol)이 만들어지고, 티올 분자는 다시 금 나노입자와 반응에 의해 티올-금 나노입자 복합체를 형성한다. 이후 신호증폭을 위해, gold(III) chloride trihydrate와 hydroxylamine hydrochloride 조합에 의한 금 나노입자의 사이즈 확대반응을 수행하였다. SAW 센서는 수용액 중에서 시안화이온에 대한 검출 능력이 17.7 uM이었으며, 공진주파수 변화량은 시안화이온의 농도가 커지면서 포화되는 현상을 보여주었다. 한편, 제작된 SAW 센서는 시안화이온 이외의 플루오라이드(fluoride), 아세테이트(acetate), 그리고 설페이트(sulfate) 이온 등의 다른 음이온에는 전혀 반응성이 없었으며, 다른 음이온에 의한 간섭현상도 나타나지 않았다. 끝으로 모든 실험은 재현성 있는 실험 결과를 얻기 위해서 자체 제작한 유체제어 모듈과 센서를 이용하여 진행하였다.