새로운 이핵 다금속 화합물

노동윤,이하진,서은미 서울여자대학교 자연과학연구소 1999 자연과학연구논문집 Vol.11 No.-

백금과 철이 포함되는 새로운 이핵 다금속 화합물인 (dppf) Pt (deydt), (dppf) Pt (ebmdt)와 (dppf) Pt (bmddt)를 합성하여 IR, UV, 고분해능 FAB 질량분석, x-선 구조분석, 순환 전압-전류법으로 분석하였다. (dppf)Pt(ebmdt)와 (dppf)Pt(bmddt)의 순환 전압-전류법 분석결과 리간드의 가역적인 산화가 먼저 일어난 후 약 1.4 V에서 가역적인 〔(dppf)Pt〕^2+의 산화가 관측되었다. 그러나 (dppf)Pt(deydt) 화합물의 경우 1. 25 V에서 가역적인 〔(dppf)Pt〕^2+의 산화가 일어난 후 1. 45 V에서 리간드의 분해로 예상되는 비가역성 산화 피이크가 관찰되었다. (dppf)Pt(deydt) 화합물의 x-선 구조분석을 185 K의 저온에서 수행하였음에도 말단의 두 -COOCH_2CH_3 기 가운데 하나가 심하게 disorder되어 있는 것으로 분석되었다. New platinum(Ⅱ) complexes, (dppf)Pt(deydt), (dppf)Pt(ebmdt) and (dppf)Pt(bmddt)(dppf: 1,1'-bis(diphenylphosphino) ferrocene; deydt: diethylester ylidenedithiolate; ebindt: 1,2-ethylenebis(methylester)-1,2-dithiolate; bmddt:5,6-bis(methylester)-1,4-dithiin-2,3-dithiolate) were synthesized and analyzed by FT-IR, UV-vis, high-resolution FAB Mass, SEM and cyclic voltammetry. Single crystal of (dppf)Pt(deydt)·(CH_3OH) was grown in dichloromethane/methanol, the molecular structure of which was clucidated by x~ray structure analysis. Crystal data at 185±2 K are a=10.6290(4), b=23.3624(10), c=17.5956(7) Å, β=105.8930(10)°, P2(1)/c, V=4202.3(3) Å^3, Z=5, R=0.0819 and wR=0.1988. According to the cyclic voltammetry, ligand oxidation occurred at lower potential than that of [(dppf)Pt]^2 for (dppf)Pt(ebmdt) and (dppf)Pt(bmddt), however, [(dppf)Pt]^2 oxidation was followed by the ligand decomposition for (dppf)Pt(deydt) complex.

유기전자물질의 전구체인 (±)-4,5-phenylethylenedithio-1,3-dithiole-2-thione의 새로운 합성법과 그 이용

노동윤,이하진 서울여자대학교 자연과학연구소 1995 자연과학연구논문집 Vol.6 No.-

A precursor to organic electronic materials, (±)-4,5-phenylethylenedithio-1,3-dithiole-2-thione, was synthesized by the direct thermal reaction of loigomeric 1,3-dithiole-2,4,5-trithione, which was easily prepared by iodine oxidation of (TBA)_2[Zn(dmit)_2] in acetone, and styrene. This reaction is proceeded via [2+4] cycloaddition between oligomeric diene and styrene as a dienophile. Compared with the salt elimination method reported already, this new pathway saves more than one reaction step and deals with relatively inert material, 1,3-dithiole-2,4,5-trithione, to moisture and common organic solvents. It is also revealed that this compound can be used as a ligand of metal coordinated complex such as Ni(phdt)_2.

자기조립 단분자막(SAM) 제작에 사용할 티올 유도체의 합성과 분석

노동윤 서울여자대학교 자연과학연구소 2001 자연과학연구논문집 Vol.13 No.-

Dodecanethiol derivative of 1,3-dithiole-2-thione (HSC12MT-DTT) has been synthesized to be used in the developement of functional self-assembled monolayer (SAM). This thiol compound is characterized by IR and 1H-/13C-NMR. Its electrochemical properly is also investigated by cyclic voltammetry.

소중합 디엔체인 1,3-dithiole-2,4,5-trithione의 Diels-Alder 형태의 [2+4] 고리화 첨가 반응에 관한 연구

노동윤,이하진,김영윤 서울여자대학교 자연과학연구소 1997 자연과학연구논문집 Vol.8 No.-

A Diels-Alder type [2+4] cycloaddition reaction of oligomeric diene (1,3-dithiole-2,4,5-trithione : (C3S5)n) with dienophiles containing warious functional groups was studied. Extended multisulfur system was achieved via [2+4] cycloaddition of TTF(1). Quinone(4), dienophiles containing cyanyl group(5-7), triple bond(14-17) and conjugated double bonds (25,26), however, failed to form cycloadducts with (C3S5)n. the reaction of (C3S5)n with dienophiles containing electron withdrawing groups such as -Co2CH3(18), phenyl(19-24), ferrocenyl(27,28), pyridyl(29,32) group was readily achieved. In case of asymmetrical dienophiles such as 19, 27, 29 and 30, the electron withdrawing ability was more efficient than symmetric dienophiles. Dienophiles of 4-vinyl pyridine group(30,32) were more reactive than that of 2-vinyl pyridine group(29,31). This reaction also could be carried out by photoreaction as well as direct thermal reaction. Eventhaugh we observed no reaction between 6 and (C3S5)n by direct thermal method, it yielded some cycloadduct via photoreaction even in very low yield. The cycloadducts, EDT-DTT derivatives, were converted to EDT-DTO derivatives using Hg(OAc)2 in CHCI3. The EDT-DTT(O) DERIVATIVES can be good can-didates as precursors to organic electronic materials.

다황리간드를 갖는 새로운 니켈 착화합물의 합성과 전기 화학적 특성 연구 : (TPP) [Ni(dmbit)₂](TPP : tetraphenylphosphonium) (TPP) [Ni(dmbit)₂](TPP : tetraphenylphosphonium)

노동윤,강미정 서울여자대학교 자연과학연구소 1995 자연과학연구논문집 Vol.6 No.-

A new nickel complex with multisulfur ligand, (TPP) [Ni(dmbit)_2] where TPP is tetraphenylphosphonium and dmbit is dimercaptobenzene isotrithione, has been synthesized from (TPP) [Ni(dmbit)_2] by cation exchange reaction and successive oxidation step by both chemical and electrochemical methods. In the electrochemical method, microcrystals of monocationic complex were grown on the surface of platinum(+) electrode while polycrystals of dicationic one were on the (+) cell bottom. That is, two reaction processes(cation exchange by diffusion and electrochemical oxidation) were occurred simultaneously in one electrochemical cell. The cyclic voltamogram of dicationic TPP-complex shows two reversible curves at 36mV and 432mV upon reduction processes of [Ni (dmbit)_2]^2- → [Ni (dmbit)_2]^1- and [Ni (dmbit)_2]^1- → [Ni (dmbit)_2]^0, respectively. The potential difference (△E1/2=396mV) of this complex exceeds those of TBA-salts and Ni-dmit complexes, which means that TPP-salt might be inferior in electrical conductivity to TBA-salt as well as Ni-dmbit complex to Ni-dmit one in general.

새로운 이핵 백금-디티올렌 화합물의 합성과 확인

노동윤,서은미,이명환 서울여자대학교 자연과학연구소 1997 자연과학연구논문집 Vol.8 No.-

중성 리간드인 dppf를 사용하여 새로운 백금 화합물을 합성하고 적외선과 자외선 분광법에 의해서 분석하였다. 적외선 분광법에 의해서 페닐기의 방향족 C=C의 신축진동이 1600cm-1~1400cm-1에서 확인되었으며, dmit 화합물에서는 1053.2cm-1에서 C=S 신축진동이, i-mnt 화합물에서는 2210.6cm-1에서 C=N 신축진동이 확인되었다. 자외선 분광법에 의해서는 400nm~500nm에서 매우 약한 페로센의 d-d 전자전이를 보였다. 또한 dmit 화합물에서 C=S의 전자전이가 466nm에서 관측되었다. New platinum(II) complexes containing 1.1'-bis(diphenylphosphino) ferrocene (dppf) as a neutral ligand and 1.2-dithiolenes (dmit : dimercapto isotrithione; dddt : 5.6-dihyro-1.4-dithiin-2.3-dithiolate; phdt : 5-phenyl-6-hydro-1.4-dithiin-2.3-dithiolate; dphdt :5.6-diphenyl-1.4-dithiin-2.3-dithiolate; mtdt : 1.2-bis(methylthio)ethylene-1.2-dithiolate) or 1.1-dihiolene (i-mnt : isomalononitriledithiolate) were synthesized in three-solvent system (benzene : methanol : water = 1 : 1 : 1). The single crystals were grown by diffusion method using dichloromethane and methanol in freezer. These compounds were characterized by FT-IR and UV-vis spectroscopic methods : In the FT-IR spectra, aromatic C=C stretching vibrations near 690~750cm-1 were observed in all Pt(dithiolene)(dppf) complexes. C=S stretching vibration of dmit ligand and C=N i-mnt ligand were also indexed at 1053.2cm-1 and 2210.6cm-1, respectively. electronic transition of phenyl group was observed between 215nm and 260nm while electronic absorption characteristic of C=S in dmit ligand appeared at 466nm in UV-vis spectra.

로손시약과 1,8-디케톤 화합물의 이상 반응

노동윤,이하진,김영윤 서울여자대학교 자연과학연구소 1997 자연과학연구논문집 Vol.9 No.-

The new 1,3-dithiole-2-thione compound fused with diphenyl-containing ?? was synthesized by an unusual reaction of Lawesson's reagent ?? with 1,8-diketone and identified with FT-lR, El-MS and ^l3C-NMR. The reaction of Lawesson's reagent and diketone compounds gives different results depending on the property of functional group at a-position of ketone. This method can be developed as a new synthetic method of multisulfur compound which may be utilized as a precursor of organic conductors. Compound ?? will be a good candidate for the precursor of new TTF derivatives, too.

제2형 당뇨병 환자에서 적극적 환자 교육이 혈당조절에 미치는 효과

이윤욱,황원선,최선정,이동훈,김도현,이은희,홍은경,노혜림,정윤석,이관우,김현만 대한내분비학회 2003 Endocrinology and metabolism Vol.18 No.1

연구배경: 현재까지의 당뇨병 교육에 대한 노력은 제한되었으며, 연구 결과를 보면 식사 조절 교육과 체중 조절 프로그램을 수행한 환자들 중 적극적이고 기간이 긴 교육을 받은 경우, 성공적 결과가 나타남을 알 수 있었다. 자가관리나 체중감량 등의 당뇨병 치료의 중요한 목표는 적극적이고 긴 기간의 교육 없이는 시행되기 어렵다. 본 연구에서는 외래에서 당뇨병 환자를 대상으로 시행할 수 있는 행동 및 식사 교육 등의 적극적 교육 프로그램을 개발하여 제2형 당뇨병 환자들을 대상으로 이들에게 식사 조절 방법에 대한 목표설정과 문제에 직면하였을 때의 해결 방법 등을 교육해서 궁극적으로는 적극적 자아관리에 연결될 수 있도록 도와주는 것을 목적으로 기존의 통상적 교육과 보다 적극적인 교육이 당뇨병 환자의 혈당 조절에 어떠한 영향을 미치는지에 대해 알아보기 위해 다음과 같은 연구를 시행하였다. 방법: 본 연구는 아주대학교 병원 내분비 대사 내과를 처음으로 방문하여 치료받았던 58명의 제2형 당뇨병 환자를 대상으로 하였다. 내원 환자들을 무작위하게 추출하여 진찰권 번호 끝자리에 따라 홀수는 통상적 교육군(conventional education group, CE)과 짝수는 적극적 교육군(intensive education group, IE)으로 나누어 교육하고, 3개월후에 교육의 효과를 평가하였다. 결과: 1) 연구 대상자들의 교육 전과 후의 공복혈당, 식후2시간 혈당 및 HbA_lc 치는 IE군과 CE군 모두 각 그룹 내에서, 유의적으로 감소하였다(p<0.05). IE군에서는 공복혈당이 12.4nmol/L에서 7.7nmol/L로, 식후2시간 혈당이 20.3nmol/L에서 10.9nmol/L으로, HbA_lc치가 9.4%에서 7.0%로 모두 교육 전에 비하여, 교육 후에 감소(p<0.05)하였고, CE군도 공복혈당은 10.9nmol/L에서 9.4nmol/L로, 식후2시간 혈당은 17.1nmol/L에서 14.6nmol/L으로 HbA_lc가 8.5%에서 7.3%으로 모두 교육 후에 감소하였다(p<0.05). 또한, 교육 전에 비하여 교육 후에 공복 혈당 및 HbA_lc치가 감소하는 정도는 IE군에서의 감소가 CE군에 비해 더 현저하였다Op<0.05). 2) 식사에 대한 태도는 3부분으로 나누어 식사에 대한 규칙성, 식사 내용의 균형성, 식사에 대한 태도 등으로 나누어 각각의 점수 및 총점을 비교하였으며 교육 전에 비해 교육 후에 연구 대상자들의 식태도가 향상되었음을 알 수 있었다. 두 그룹간의 차이를 분석한 결과 식사의 균형성 항목에서와 총점에서 유의적으로 두 그룹의 차이를 보여서 IE군에 CE군에 비해 식사의 균형성 측면이 향상되었고, 전체적인 식태도가 좋아졌음을 알 수 있었다(p<0.05). 결론: 비교적 긴 기간은 아니지만 적극적 교육을 받은 당뇨병 환자들이 통상적 교육을 받은 군보다 혈당 및 HbA_lc, 식태도 점수등의 수치의 호전뿐만 아니라 당뇨병 환자의 삶에서 중요한 부분을 차지하는 식사요법 관리 부분에 있어 향상됨을 알 수 있었다. Background: To this date, efforts to develop effective methods for the education of diabetic patients have been limited. The important goal of self-management and weight control for diabetic treatment can not be attained without long and intensive period of education. This study was undertaken to assess the effectiveness of an intensive educational program, of behavior and diet control, which was carried out on subjects with type 2 diabetes, on and out-patient basis. we compared the effectiveness of an intensive education programme with that of a conventional education programme for the self-management of type 2 diabetic patients. Methods: Subjects with type 2 diabetes were randomly selected, and allocated to one of two groups. One group received a conventional education programme of self-management(the CE group), and the second group received an intensive education progammes for three months, after which the effectiveness of the programmes were evaluate. Results: 1) The levels of fasting blood sugar(FBS), postprandial 2 hour blood sugar(PP2h) and HbA1c were significantly lowered in both groups following the intervention(p<0.05). In the IE group, the FBS declined from 12.4nmol/L to 7.7nmol/L, PP2h declined from 20.3nmol/L to 10.9nmol/L, and the HbA_lc showed a similar decline from 9.4 to 7.0% after intervention(p<0.05). In the Ce group, the FBS declined from 10.9 to 9.4nmol/l, the PP2h decreased from 17.1 to 14.6nmol/l, and the HbA_lc also decreased from 8.5 to 7.3% after intervention(p<0.05). The decrease in the FBS and HbA_lc following the educational intervention was more pronounced in the IE group than the CE group(p<0.05). 2) The effectiveness of the education programmes in promoting appropriate dietary behavior in the diabetic subjects was assessed by a scoring system in three parts: a regularity score, a balance score and an attitude score. From a comparative study of the three scores, the patients attitudes were observed to be much improved in both the groups following the intervention compared to before the programmes, but the balance and total scores were significantly higher in the IE group than the CE group(p<0.05). Conclusion: We can conclude that the intensive diabetic education programme is more effective than a conventional programme, not only in improving the patients' levels of glucose, HbA_lc, and dietary score, but also the diabetic patients self-control abilities, promoting behavioral change, and prompting problem solving capabilities in respect to the everyday problems that they have to face throughout their lives(J Kor Soc Endocrinol 18:63∼72, 2003).

피리딘으로 연결된 이핵 팔라듐(II) 또는 백금(II) 자기조립 화합물

신경순,노동윤 서울여자대학교 자연과학연구소 2006 자연과학연구논문집 Vol.18 No.-

As a challenge for the molecular engineering of metal-coordinated self-assembly, Pd(II) and Pt(II) building blocks containing 1,2-bis(diphenylphosphino) acetylene (dppa) bridging ligand are treated with ditopic organic linkers such as pyridine derivatives and ethylenediamine (en). The polymeric metal-coordinated complexes are characterized by FT-IR and CHSN elemental analysis. The possible coordination modes are suggested on the basis of the analytical data. 여러 가지 피리딘 유도체와 ethylene-diamine을 organic linker로 하고 M_(2)(OTf)_(4) (^(μ) -Ph_(2)PC=CPPh_(2))_(2)를 단위체로 하여 자기 조립 복합체를 확산반응을 통하여 합성하였다. 합성된 자기조립 화합물은 FT-IR, CHSN 원소분석으로 그 특성을 관찰하였다. FT-IR 분광분석으로 화합물들에 포함되어 있는 피리딘 유도체들의 C=C와 C=N 진동 패턴이 순수한 피리딘 분자의 그것과 동일 하지 않고 단위체가 포함하는 금속의 종류에 따라서 그 정도의 차이가 있는 것으로 관찰되었다. 이것은 분자궤도함수의 겹침과 그에 따른 피리딘 유도체들의 C=C와 C=N 의 진동패턴의 변화를 설명할 수 있다.

두 가지 CET-EDTTTF 동질이상 화합물의 구조 비교

권선영,노동윤 서울여자대학교 자연과학연구소 2005 자연과학연구논문집 Vol.17 No.-

CET-EDTTTF was synthesized and crystallized (CH_(2)Cl_(2)/CH_(3)CH_(2)OH) in monoclinic system with P2(1) space group and the cell parameters: a = 5.0570(15)Å, b = 20.702(5)Å, c = 14.759(3)Å, beta = 90.30(2)°. CET-EDTTTF molecules arranged in bc-plane are stacking along the a-axis. There is no intermolecular S···S interaction shorter than the sum of the van der Waals radii of sulfur atom(3.70Å). When CET-EDTTTF was reacted with AgCF_(3)SO_(3), black single crystals of (CET-EDTTTF)·(solv) were obtained after crystallization. It crystallized in triclinic system with P-1 space group and the cell parameters: a = 6.5962(14)Å, b = 9.123(2)Å, c = 15.545(3)Å, alpha = 77.491(3)°, beta = 87.646(3)°, gamma = 69.332(3)°. CET-EDTTTF molecules form dimers with head-to-tail fashion, which are stacking along b-axis. The molecular sheets formed in ab-plane are separated by the solvated molecules. The CET-EDTTTF molecules in this sheet are connected by the intermolecular S···S interactions shorter than 3.70Å.