• 제목/요약/키워드: NMR

검색결과 4,953건 처리시간 0.041초

Higenamine의 합성 및 가토의 심혈관계에 미치는 영향 : 베타-아드레날린성 효능 약물 (Synthesis of Higenamine and its Cardiovascular Effects in Rabbit: Evidence for ${\beta}-Adrenoceptor$ agonist)

  • 장기철;임정규;박찬웅
    • 대한약리학회지
    • /
    • 제22권2호
    • /
    • pp.96-104
    • /
    • 1986
  • 최근에 미나라아제비과 (Ranunculaceae)에 속하는 부자(Aconiti tuber)로부터 강심작용을 나타내는 성분을 분리하여 Higenamine이라 명명하였고 그 작용기전을 밝히려는 시도가 활발히 진행되고 있다. 그러나 생약제로 부터 얻을 수 있는 Higenamine은 극히 미량이고 그 과정 또한 복잡하다. 따라서 본 연구에서는 유효성분을 대량 얻기 위한 방법으로서 전합성(total Synthesis)을 시도하였으며 IR, UV, NMR 및 elemental 분석등을 통하여 합성된 물질을 확인하였으며 가토에 대하여 in vivo에서 혈압, 심박동수, 호흡 및 말초저항에 미치는 영향과 아울러 in vitro에서 심근수축 증강작용(positive inotropic action) 및 심박속도 증강작용(positivechronotropic action)을 관찰 분석하여 다음과 같은 결론을 얻었다. 1) Higenamine은 $1-10\;{\mu}g/kg/min$ 정맥주사시 수축기 및 이완기혈압 모두를 용량 의존적으로 하강시켰고 후자가 전자보다 더욱 현저하였으며 호흡은 촉진되었고 말초 혈류량은 증가되었으나 심박동수는 영향이 없었다. 2) 혈압에 대한 Higenamine의 작용은 propranolol 전처치에 의하여 억제되었다. 3) Higenamine의 catechol핵과 커다란 아미노기는 베타 수용체기 대하여 전자는 활성을 후자는 친화력과 관계있을 것으로 추정하였다. 이상의 결과 Higenamine은 adrenergic ${\beta}$-수용체에 작용하여 그 작용을 발휘하는 것으로 사료 되었다.

  • PDF

Halogen-Free 난연제를 포함하는 파우더 코팅소재 제조 및 화재안전성 연구 (A Study on the Preparation of Powder Coatings Containing Halogen-Free Flame Retardant and Fire Safety)

  • 이순홍;정화영;김대인;노태준
    • 한국안전학회지
    • /
    • 제26권4호
    • /
    • pp.47-58
    • /
    • 2011
  • Halogen free intumescent flame retardants(IFRS), such as the mixture of melamine phosphate(MP) and char forming agents(pentaerythritol(PER), di-pentaerythritol(DiPER), tris(2-hydroxyethyl) isocyanurate(THEIC)), were prepared and characterized. Polypropylene(PP)/$IFR_S$ composites were also prepared in the presence of ethylene diamine phosphate(EDAP) as a synergist and used into flame retardant PP powder coatings. Thermoplastic PP powder coatings at 20 wt% flame retardant loading were manufactured by extruded and then mechanical cryogenic crushed to bring them in fine powder form. These intumescent flame retardant powder coatings($IFRPC_S$) were applied on mild steel surface for the purpose of protection and decorative. It is a process in which a $IFRPC_S$ particles coming in contact with the preheated mild steel surface melt and form a thin coating layer. The obtained MP flame retardant was analyzed by utilizing FTIR, solid-state $^{31}P$ NMR, ICP, EA and PSA. The mechanical properties as tensile strength, melt flow index(MFI) and the thermal property as TGA/DTA and the fire safety characteristics as limiting oxygen index(LOI), UL94 test, SEM were used to investigate the effect of $IFRPC_S$. The experimental results show that the presence of $IFR_S$ considerably enhanced the fire retardant performances as evidenced by the increase of LOI values 17.3 vol% and 32.6 vol% for original PP and $IFRPC_S$-3(PP/MP-DiPER/EDAP), respectively, and a reduction in total flaming combustion time(under 15 sec) in UL94 test of $IFRPC_S$. The prepared $IFRPC_S$-3 have good comprehensive properties with fire retardancy 3.2 mm UL94 V-0 level, LOI value 32.6%, tensile strength $247.3kg/cm^2$, surface roughness Ra $0.78{\mu}m$, showing a better application prospect. Through $IFRPC_S$-2(PP/MP-PER/EDAP) and $IFRPC_S$-3 a better flame retardancy than that of the $IFRPC_S$-1(PP/MP/EDAP) was investigated which was responsible for the formed more dense and compact char layer, improved synergy effect of MP and PER/DiPER.

Copolymerization of Ethylene and Norbornene via Polymethylene Bridged Dinuclear Constrained Geometry Catalysts

  • Zhu, Yin-Bang;Jeong, Eung-Yeong;Lee, Bae-Wook;Kim, Bong-Shik;Noh, Seok-Kyun;Lyoo, Won-Seok;Lee, Dong-Ho;Kim, Yong-Man
    • Macromolecular Research
    • /
    • 제15권5호
    • /
    • pp.430-436
    • /
    • 2007
  • The dinuclear half-sandwich CGCs (constrained geometry catalyst) with a polymethylene bridge, $[Ti({\eta}^5 : {\eta}^1-indenyl)SiMe_2NCMe_3]_2(CH_2)_n]$[n = 6 (1) and 12 (2)], have been employed in the copolymerization of ethylene and norbornene (NBE). To compare the mononuclear metallocene catalysts; $Ti({\eta}^5 : {\eta}^1-2-hexylindenyl)SiMe_2NCMe_3$ (3), $(Cp^* SiMe_2NCMe_3)$Ti (Dow CGC) (4) and ansa-$Et(Ind)_2ZrCI_2$ (5), were also studied for the copolymerization of ethylene and NBE. It was found that the activity increased in the order: 1 < 2 < 3 < 5 < 4, indicating that the presence of the bridge between two the CGC units contributed to depressing the polymerization activity of the CGCs. This result strongly suggests that the implication of steric disturbance due to the presence of the bridge may playa significant role in slowing the activity. Dinuclear CGCs have been found to be very efficient for the incorporation of NBE onto the polyethylene backbone. The NBE contents in the copolymers formed ranged from 10 to 42%, depending on the polymerization conditions. Strong chemical shifts were observed at ${\delta}$42.0 and 47.8 of the isotactic alternating NBE sequences, NENEN, in the copolymers with high NBE contents. In addition, a resonance at 47.1 ppm for the sequences of the isolated NBE, EENEE, was observed in the $^{13}C-NMR$ spectra of the copolymers with low NBE contents. The absence of signals for isotactic dyad at 48.1 and 49.1 ppm illustrated there were no isotactic or microblock (NBE-NBE) sequences in the copolymers. This result indicated that the dinuclear CGCs were effective for making randomly distributed ethylene-NBE copolymers.

Bacillus subtilis GDYA-1로부터 분리한 benzoic acid의 식물병원성 곰팡이에 대한 항균활성 (Antifungal Activity of Benzoic Acid from Bacillus subtilis GDYA-1 against Fungal Phytopathogens)

  • 윤미영;서국화;이상현;최경자;장경수;최용호;차병진;김진철
    • 식물병연구
    • /
    • 제18권2호
    • /
    • pp.109-116
    • /
    • 2012
  • 전라남도 영남지역의 감나무 줄기로부터 다양한 식물병에 대해 방제 효과를 보이는 세균을 분리하였다. 분리균주는 16S rRNA sequencing의 방법을 이용하여 동정한 결과 B. subtilis로 동정되었으며, B. subtilis GDYA-1로 명명하였다. In vivo 생물검정에서 GDYA-1 액체 배양액은 벼 도열병, 토마토 역병 및 밀 붉은녹병에 항균 활성을 보였다. 액체 배양액으로부터 한 개의 항균물질을 분리하였으며, 질량분석과 핵자기공명분석을 통해 분리한 물질은 benzoic acid로 동정되었다. Benzoic acid는 M. oryzae, R. solani, S. sclerotiorum 및 P. capsici의 균사생육을 62.5-125 ${\mu}g/ml$에서 완전히 억제하였다. 또한 benzoic acid는 고추 역병을 효과적으로 방제하는 것으로 나타났다. 본 연구에서 benzoic acid의 식물병원성곰팡이에 대한 항균활성을 처음으로 보고하는 바이다. Benzoic acid와 B. subtilis GDYA-1는 식물병원성곰팡이로부터 작물을 친환경적으로 보호하는데 기여할 것으로 기대된다.

천연인디고 색소의 구조분석 (Structural Analysis of Natural Indigo Colorants Extracted from Polygonum tinctorium)

  • 정인모;이광길;성규병;김현복;남성희;홍인표
    • 한국잠사곤충학회지
    • /
    • 제49권1호
    • /
    • pp.8-13
    • /
    • 2007
  • 쪽풀 생잎에서 우려낸 색소 액에 소석회를 첨가한 후 쪽풀 색소의 침전물을 만들어서 냉동 건조시켜 쪽풀 색소를 제조하여, 그 성분을 조사한 결과 다음과 같은 결론을 얻었다. 1. UV분광광도, TLC 정성 분석, HPLC 측정 결과 쪽 분말 용액의 2개 bend가 나타났으며, 적색색소대인 540nm 와 청색 색소대인 620nm가 존재함을 알 수 있었다. 2. FT-IR 분석으로부터 $1627cm^{-1}$에서 채, $3200{\sim}3300cm^{-1}$에서 NH의 흡수대가 나타나고, 적색 및 청색 색소의 IR spectrum이 일치하였으며, 3. EI-mass 분석 결과 청색과 적색 색소의 fragment 이온의 m/z가 일치하고, $^1H_MNR$ 분석결과로부터 두 색소는 이성질체임을 알 수 있었고, 4. 쪽 염료 성분 함량을 조사한 결과 인디고 색소 4.06%와 인디루빈 1.06%이었다.

무 시들음병균이 생산하는 Phytotoxin의 병원성 및 저항성에서 역할 (Role of a Phytotoxin Produced by Fusarium oxysporum f. sp. raphani on Pathogenesis of and Resistance to the Fungus)

  • 심선아;김진철;장경수;최용호;김흥태;최경자
    • 원예과학기술지
    • /
    • 제31권5호
    • /
    • pp.626-632
    • /
    • 2013
  • 무 시들음병에 대한 저항성 검정 체계를 확립하기 위하여 실험하는 과정에서 병원균인 Fusarium oxysporum f. sp. raphani가 무 유묘에 독성(phytotoxicity)을 일으키는 독소(phytotoxin)를 생산한다는 것을 발견했다. F. oxysporum f. sp. raphani KR1 균주는 여러 배지 중 malt extract broth 배지에서 배양하였을 때 그리고 $25^{\circ}C$에서 14일 동안 150rpm으로 진탕배양하였을 때 가장 많은 독소를 생산하였다. 무에 대한 독성 반응을 이용하여 F. oxysporum f. sp. raphani의 배양액으로부터 phytotoxin을 분리하였다. 그리고 Mass와 NMR Spectroscopy 분석을 통하여 이 화합물은 fusaric acid로 동정되었다. 독소의 역할을 규명하기 위하여 fusaric acid를 무, 양배추, 브로콜리 등 F. oxysporum f. sp. raphani의 기주 및 비기주 배추과 작물에 대한 독소 활성을 조사하였다. Fusaric aicd는 무 유묘에 대하여 농도 의존적으로 활성을 보였으며, F. oxysporum f. sp. raphani에 대한 감수성 품종뿐만 아니라 저항성 품종에 대해서도 유사한 정도의 독성을 나타냈다. 그리고 F. oxysporum f. sp. raphani가 생산하는 fusaric acid는 병원균의 비기주 배추과 작물인 양배추와 브로콜리에 대해서도 강한 활성을 보였다. 따라서 이들 결과는 이 독소가 병원성 관련 독소이나 비기주 특이적 독소이며, 무 시들음병 저항성 검정에서 이 독소가 제거된 포자현탁액을 접종원으로 사용해야 한다는 것을 나타낸다.

Interaction of the Post-transition Metal Ions and New Macrocycles in Solution

  • Jung, Oh-Jin
    • Bulletin of the Korean Chemical Society
    • /
    • 제14권6호
    • /
    • pp.687-691
    • /
    • 1993
  • Complexation of $Cd^{2+},\;Pb^{2+}\;and\;Hg^{2+}$ ions with four cryptands were studied by potentiometry and solution calorimetry in various weight percent methanol-aqueous solvent at 25${\circ}$C under $CO_2$free nitrogen atmosphere. The stabilities of the complexes were dependent on the cavity size of macrocycles. The $Hg^{2+}$ ion stability constants are higher than those of $Cd^{2+}\;and\;Pb^{2+}$ ion. All the cryptands formed complexes having 1 : 1 (metal to ligand) mole-ratio except for $Hg^{2+}-L_1$ (cryptand 1,2b: 3,5-benzo-9,14,17-trioxa-1,7-diazabicyclo-(8,5,5) heptadecane) and $Cd^{2+}-L_2$ (cryptand 2,2b: 3,5-benzo-10,13,18,21-tetraoxa-1,7-diazabicyclo (8,5,5) eicosane) complexes. $Hg^{2+}-L_1$ complex was a sandwitch type, and the $Cd^{2+}-L_2$ complex showed two stepwise reactions. Thermodynamic parameters of the $Cd^{2+}-L_2$ complex were $6.08(log\;K_1)$, -7.28 Kcal/mol $({\Delta}H_1)$, and $4.78\;(log\;K_2)$, -4.62 Kcal/mol $({\Delta}H_2)$, respectively, for 1 : 1 and 2: 1 mole-ratio. The sequences of the selectivity were increased in the order of $Hg^{2+}\;>Pb^{2+}\;>Cd^{2+}$ ion for $L_3\;and\;L_4$ macrocycles, and the $L_2$-macrocycle has a selectivity for $Cd^{2+}$ ion relative to $Zn^{2+},\;Ni^{2+},\;Pb^{2+}\;and\;Hg^{2+}$ ions. Thus, it is expected that the $L_2$ can be used as carrier for seperation of the post transition metals by macrocycles-mediated liquid membrane because $L_2$ is not soluble in water, and the difference of stability constants of the metal complexes with $L_2$ are large as compared with the other transition metal complexes. The $^1H\;and\;^{13}C-NMR studies indicated that the nitrogen atoms of cryptands have greater affinity to the post transition metal ions than the oxygen atoms, and that the planarities of the macrocycles were lost by complexation with the metal ions because of the perturbation of ring current of benzene molecule attached to macrocycles and counter-anions.

Efficient Synthesis of hypho-2,5-$S_2B_7H_{11}$ and Preparation of New nido-, arachno-, and hypho-Metalladithiaborane Clusters Derived from Its Anion hypho-$S_2B_7H_{10}{^-}$

  • 강창환;김성준;고재정;강상욱
    • Bulletin of the Korean Chemical Society
    • /
    • 제16권11호
    • /
    • pp.1067-1074
    • /
    • 1995
  • Reaction of arachno-S2B7H8- with either THF or 1,2-dimethoxyethane upon refluxing condition results in the formation of the previously known compound hypho-S2B7H10-. Protonation of hypho-S2B7H10- with HCl/Et2O generates hypho-2,5-S2B7H11 in good yield. This hypho-S2B7H10- anion has been employed to generate a series of new nido-, arachno-, and hypho-metalladithiaborane clusters. Reaction of the anion with Cp(CO)2FeCl results in direct metal insertion and the formation of a complex containing the general formula (η5-C5H5)FeS2B7H8. Spectroscopic studies of nido-6-CpFe-7,9-S2B7H8 Ⅰ demonstrated that compound Ⅰ was shown to have an nido-type cage geometry derived from an octadecahedron missing one vertex, with the iron atom occupying the three-coordinate 6-position in the cage and the two sulfurs occupying positions on the open face of the cage. Reaction of hypho-S2B7H10- with CoCl2/Li+[C5H5]- gave the previously known complex arachno-7-CpCo-6,8-S2B6H8 Ⅱ. Also, the reaction of the anion with [Cp*RhCl2]2 gave the complex arachno-7-Cp*Rh-6,8-S2B6H8 Ⅲ, the structure of which was shown to be that of complex Ⅱ. The similarity of the NMR spectra of Ⅱ and Ⅲ suggest that Ⅲ adopts cage structure similar to that previously confirmed for Ⅱ. A series of 9-vertex hypho clusters in which the sulfur atoms are bridged by different species isoelectronic with a BH3 unit, such as HMn(CO)4 or SiR2 have been prepared. Compounds Ⅳ,Ⅴ and Ⅵ are each 2n+4 skeletal electron systems and would be expected according to skeletal electron counting theory to adopt hypho-type polyhedral structures derived from an icosahedron missing three vertices. The complex hypho-1-(CO)4Mn-2,5-S2B6H9 Ⅳ was obtained by the reaction of the anion with (CO)5MnBr and has been shown from spectroscopic data to consist of a (CO)4Mn fragment bound to the two sulfur atoms S2 and S5 of hypho-S2B7H10-. Also, similar hypho-type complexes hypho-1-R2Si-2,5-S2B6H8 (R=CH3 Ⅴ, R=C6H5 Ⅵ) have been prepared from the reaction of hypho-S2B7H10- with R2SiHCl.

Proliferative Effects of Flavan-3-ols and Propelargonidins from Rhizomes of Drynaria fortunei on MCF-7 and Osteoblastic Cells

  • Chang, Eun-Ju;Lee, Won-Jung;Cho, Sung-Hee;Choi, Sang-Won
    • Archives of Pharmacal Research
    • /
    • 제26권8호
    • /
    • pp.620-630
    • /
    • 2003
  • The proliferative effects of thirty Oriental medicinal herbs on MCF-7 (estrogen-sensitive breast cancer cell line) and ROS 17/2.8 osteoblast-like cells were determined using the MTT assay. Methanol extracts from several herbs was found to show proliferative activity on the above two cell lines in the range of 5 to 100 $\mu$g/mL. Among these active herbs, the methanol extract from the rhizomes of Drynaria fortunei showed the most potent proliferative activity, and the cell proliferations were significantly increase by 136 and 158% in the MCF-7 and ROS 17/2.8 cells, respectively, when treated with 100 $\mu$ g/mL. Through a bioassay-guided separation, eight flavonoids, including four new flavan-3-ols and two propelargonidins, together with the known (-)-epiafzelechin and naringin, were isolated. Their chemical structures were characterized as (-)-epiafzelechin (1), (-)-epiafzelechin-3-O-$\beta$-D-allopyranoside (2), (-)-epiafzelechin-3-O-(6"-O-acetyl)-$\beta$-D-allopyranoside (3), 4$\beta$-carboxymethyl-(-)-epiafzelechin methyl ester (4), 4$\beta$-car-boxymethyl-(-)-epiafzelechin sodium salt (5), naringin (6), (-)-epiafzelechin-(4$\beta$\rightarrow8)-4$\beta$-car-boxymethylepiafzelechin methyl ester (7) and (-)-epiafzelechin-($4\beta\rightarrow8, 2\beta\rightarrowΟ\rightarrow7)-epiafzelechin-(4\beta\righarrow8)-epiafzelechin (8) by extensive 1D and 2D NMR spectroscopy. Most of these flavonoids, in the range of $10^{-15}∼10^{-6}$ M, accelerated the proliferation of MCF-7 cell, with compounds 7 and 8, in the range of $10^{-15}∼10^{-12}$ M, showing especially potent proliferation effects. Meanwhile, seven flavonoids, with the exception of compound 4, stimulated the proliferation of ROS 17/2.8 cells in the range of $10^{-15}∼10^{-6}$ M, with compounds 5-8 especially accelerating the proliferation, in dose-dependent manners ($10^{-15}∼10^{-9}$ M), and their proliferative effect was much stronger than that of $E_2$ and genistein. These results suggest that propelargonidin dimers and trimers isolated from the rhizomes of Drynaria fortunei may be useful as potential phytoestrogens, which play important physiological roles in the prevention of postmenopausal osteoporosis.

아미드 커플링을 통한 덴드리틱 Polystyrene-Block-Linear Poly(t-butyl acrylate) 공중합체의 합성 (Synthesis of Dendritic Polystyrene-block-Linear Poly(t-butyl acrylate) Copolymers by an Amide Coupling)

  • 송걸;조병기
    • 폴리머
    • /
    • 제33권2호
    • /
    • pp.158-163
    • /
    • 2009
  • 본 연구에서는 잘 정의된 덴드리틱 폴리스티렌-블록-선형 폴리(3차 부틸 아크릴레이트) 공중합체를 성공적으로 합성하였다. 음이온 중합법을 통해 합성된 폴리스티렌($M_n$=1000 g/mol)을 외곽부분으로 함유하는 덴드론의 수산기 그룹을 토실화(tosylation), 아지드화(azidation), 환원(reduction) 반응을 통해 아민기로 전환하였다. 한편, 선형 poly(t-butyl acrylate)는 DMF 용매에서 benzyl 2-bromopropanoate/Cu(I)Br, PMDETA/t-butylacrylate를 각각 개시제/촉매 시스템/단량체로 사용하여, 원자이동라디칼 중합법(atom transfer radical polymerization, ATRP)을 통해 합성할 수 있었고, 말단을 카르복시산 그룹으로 전환하기 위해 수소기체 환경하에서 Pd/C 을 사용하여 탈벤질화(debenzylation) 반응을 수행하였다. 마지막으로, 합성된 덴드리틱 및 선형 블록들을 다이메틸아미노피리딘(4-(dimethylamino)pyridine, DMAP)과 다이아이소프로필카보다이이미드(N,N'-diisopropylcarbodiimide, DIPC)를 이용한 아미드 커플링 방법을 통해 최종 덴드리틱-선형의 블록공중합체를 합성하였다. 합성된 블록공중합체를 수소원자핵공명법 및 겔침투크로마토그래피 방법을 통해 조사한 결과, 잘 정의된 분자량 및 낮은 분자량 분포를 확인할 수 있었다.