1 N, N &#39;의 합성 -. (알칸-1, N-디일) diisonicotinamide <ol><li> 모든 수분을 제거하기 위해 오븐 (100 º C, 1 시간)에서 하나의 목 또는 3 구 둥근 바닥 플라스크를 건조. </li><li> 자기 교반 막대와 함께 플라스크에 고체 이소 니코틴산, 또는 그 유도체를 추가합니다. diaminoalkane 리간드 (들)이 실온에서 고체 인 경우에, (이소 니코틴산의 숫자 몰) 0.5 몰의이 단계에서 플라스크에 첨가된다. </li><li> 고무 격막으로 플라스크의 목 (들) 모자 및 지속적인 질소 스트림을 통해 또는 질소 채워진 풍선의 사용을 통해 하나의 질소와 함께 플라스크 내에서 공기를 교체한다. </li><li> 고체를 용해 무수 디메틸 포름 아미드 또는 디메틸 술폭 시드 (아이소 니코틴산 또는 2 - 메틸 - 아이소 니코틴산 500 mg의 당 4 ㎖)에 추가하는 피하 주사 바늘 및 주사기를 사용한다. 고형물이 쉽게 용해되지 않는 경우, 상기 용액을 온화하게 가열한다. </li><li> 에 7 몰 당량 (추가트리 에틸 아민 (약 염기)과 diaminoalkane 0.5 몰 당량 사용되는 이소 니코틴산)의 산. 용액은 실온에서 액체 인 경우, 1.5 몰 당량을 추가한다. </li><li> 연속 교반하면서 1 - 프로필 포스 무수물 (커플 링제)의 1 몰 상당을 추가하고 반응이 5-12 시간에 완료 할 수 있습니다. </li></ol> 리간드 2. 정제 <ol><li> 반응이 진행됨에 따라 제품이 용액으로부터 침전에 10 개 이상의 메틸렌 그룹과 diaminoalkane 리간드를 사용하여 만든 비스 피리딘 리간드를 들어, 기다립니다. </li><li> 비스 피리딘 리간드 디아를 사용하여 제조를 들어, ~에게 물 40 ㎖를 첨가하여 생성물을 침전. </li><li> 비스 피리딘은 2-6 메틸렌 그룹의 디아 미노를 사용하여 만든 경우, 물 ~ 40 ㎖를 추가하고 화합물 1-3 일에 걸쳐 구체화 할 수 있습니다. </li><li> 진공 여과에 의해 각 비스 피리딘 리간드를 수집하고 당 200 끓는 물에 약 400 ~ 500 ㎖의 재결정리간드의 MG. 참고 : 더 많은 물이 그들의 환원수 용해도로 인해 긴 비스 피리딘 리간드 필요하다. </li><li> 화합물은 재결정시 무료 기지를 보장하기 위해 솔루션의 NaOH 및 KOH (pH가 9)를 추가합니다. </li></ol> 이핵 플래티넘 단지 3. 합성 및 정제 <ol><li> 완전 (II), transplatin은, 뜨거운 (70 ~ 80 º C에서) 물 (transplatin 200 밀리그램 당 150 ㎖)을 분명 강하게 노란색 컬러 솔루션을 생산하는 트랜스 diamminodichloridoplatinum을 녹입니다. </li><li> 비스 피리딘 리간드의 0.5 몰 상당을 추가하고 리간드 해소 (맑은 용액)까지의 온도에서 저어. 무색 근처에 설정하는 솔루션을 기다립니다 열을 끄고, 몇 가지 추가 시간 동안 실온에서 교반. </li><li> 노란 색깔의 분말을 얻을 것이다, 회전 증발에 의해 용매를 제거합니다. </li><li> 최소 따뜻한 물 양 (~ 50 &amp;에 용해하여, 백금 착물 (들)를 정화# 186, C). 남아있는 노란색 또는 흰색 컬러 고체가있는 경우, 다음이를 필터링 할 수 있습니다. </li><li> 금속 착체의 중합체 형태로 나타나며, 반응 생성물의 10 %까지 나타내는 백색 침전물이 형성 될 때까지 용액에 아세톤을 추가. 더 이상 침전물이 나타납니다 때까지 아세톤을 첨가 (~ 추가로 20 ~ 30 ㎖)을 계속합니다. 참고 :이 흰색 침전물이 불순물이다. </li><li> 나일론 여과지 (0.2 ㎛의 공극 크기) 및 순수한 생성물을 수득 할 건고 잔류 용액을 회전 증발을 통해 내용물을 여과하여 침전물을 제거한다. 주 : 필요한 경우, 추가의 아세톤 침전 단계가 복잡 순정까지 수행 될 수있다. </li></ol>

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저자가 공개하는 게 없다.

이 작품에서 이핵 백금 착물은 잠재적 인 항암제로 합성되었다. 이렇게 제조 된 비스 피리딘 가교 리간드 이소 니코틴산 및 가변 길이 디아 미노 알칸을 사용 아미드 커플 링 반응을 통해 합성 하였다. 이전에 2 ~ 8 메틸렌 그룹과 각각의 백금 착체와 비스 피리딘 리간드와 자신의 메틸 유사체의 합성이보고 된 바있다. 본 논문에서는 합성 및 정제 방법은보다 빠르고 저렴하고 개정되었습니다, 8, 10,...

백금 항암제는 인간의 암 (1)의 치료에 에이전트의 가장 널리 사용되는 제품군 중 하나 남아있다. 자신의 성공에도 불구하고, 그들은 심각한 용량 제한 부작용 2-4으로 자신의 응용 프로그램에 제한됩니다. 환자에게 투여 할 수있는 제한 용량은 종양이 저항 5를 개발할 수 있다는 것을 의미한다. 예컨대, 새로운 약물 부작용 프로파일을 개선하고 phenanthriplatin 6 및 7 phosphaplatin 같이 취득한 저항을 극복하기 위해 개발 될 계속. 1990 년대 후반, trinuclear 백금 약물, BBR3464 (반응식 1) 8, 즉 최고의 백금 약물, 시스플라틴보다 체외에서 최대 1,000 X 더 많은 세포 독성을 개발했다. BBR3464 또한 인간 암 세포주 15의 패널에서 취득한 저항을 극복 할 수있다. 불행하게도, BBR3464의 증가 된 활동은 50 일치 - 100 - 높은 독성을 배하는10-12의 사용을 제한합니다. 그것은 또한 쉽게 ​​약물의 작은 의미, 몸에서 분해되어 9 그대로 암 핵에 도달한다. Picoplatin는 2 - 메틸 - 피리딘 리간드 (반응식 1) (13)를 포함 단핵 백금 계 약물이다. 본제의 메틸기 생물학적 친핵체에 의한 공격으로부터 보호; 특히 시스테인 및 펩타이드 / 단백질 14 ~ 16가 포함 된 메티오닌. 이와 같이, 약물은 매우 안정되어 BBR3464 및 시스플라틴 (17) 모두와 비교하여 암 핵 도달 훨씬 높은 농도를 갖는다. 그 감소 된 반응성도 picoplatin가 BBR3464 및 시스플라틴 10,18,19에 비해 높은 최대 허용 선량을 의미합니다. 이 프로젝트는 따라서 개선 된 생물학적 안정성과 덜 심각한 측면 EFFE을 표시 인수 저항을 극복 할 수있는 새로운 약물을 생산하기 위해 BBR3464 및 picoplatin의 속성을 결합하는 노력CTS (예를 들어, 그림 1). 이 과정에서, 이핵 백금 착체의 범위는 가교 된 비스 피리딘 리간드와 20을 제조 하였다. 리간드 아이소 니코틴산 또는 2 - 메틸 - 아이소 니코틴산, 가변 길이 디아 미노 알칸 같은 그 유도체와의 아미드 커플 링 반응을 사용하여 제조된다. transplatin 두 몰 당량 리간드의 1 몰 상당의 반응은 원하는 백금 착물 (반응식 1)를 산출한다.

<table border="0" cellpadding="0" cellspacing="0" width="782">
	<tbody>
		<tr height="24">
			<td height="24" style="height:24px;width:297px;">D2O</td>
			<td style="width:175px;">Aldrich</td>
			<td align="right" style="width:159px;">151882</td>
			<td style="width:152px;">99.9% D</td>
		</tr>
		<tr height="24">
			<td height="24" style="height:24px;width:297px;">DMSO-d6</td>
			<td style="width:175px;">Aldrich</td>
			<td align="right" style="width:159px;">156914</td>
			<td style="width:152px;">99.96% D</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:297px;">1,8-diaminooctane</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">D22401</td>
			<td align="right" style="width:152px;">98%</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:297px;">1,10-diaminodecane</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">D14204</td>
			<td align="right" style="width:152px;">98%</td>
		</tr>
		<tr height="80">
			<td height="80" style="height:80px;width:297px;">1,12-diaminododecane</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">D1,640-1</td>
			<td align="right" style="width:152px;">98%</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:297px;">Isonicotinic acid</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">I17508</td>
			<td align="right" style="width:152px;">99%</td>
		</tr>
		<tr height="120">
			<td height="120" style="height:120px;width:297px;">1-Propylphosphonic anhydride solution</td>
			<td style="width:175px;">Aldrich</td>
			<td align="right" style="width:159px;">431303</td>
			<td style="width:152px;">50 wt% in ethyl acetate</td>
		</tr>
		<tr height="100">
			<td height="100" style="height:100px;width:297px;">Trans-diaminodichloridoplatinum(II)</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">P1525</td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Dimethylsulfoxide</td>
			<td style="width:175px;">Sigma-Aldrich</td>
			<td style="width:159px;">Z76855</td>
			<td style="width:152px;">&#62;99.9%, anhydrous</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">N,N&#8217;-dimethylformamide</td>
			<td style="width:175px;">Sigma-Aldrich</td>
			<td align="right" style="width:159px;">227056</td>
			<td style="width:152px;">99.8%, anhydrous</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Triethylamine</td>
			<td style="width:175px;">Sigma-Aldrich</td>
			<td style="width:159px;">T0886</td>
			<td style="width:152px;">&#62;99%</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Nylon filter membranes</td>
			<td style="width:175px;">Whatman</td>
			<td style="width:159px;">7402-004</td>
			<td style="width:152px;">Pore size, 0.2 &#181;m</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Equipment</td>
			<td style="width:175px;"></td>
			<td style="width:159px;"></td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Magnetic stirring hotplate</td>
			<td style="width:175px;"></td>
			<td style="width:159px;"></td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Magnetic stirring bar&#160;</td>
			<td style="width:175px;"></td>
			<td style="width:159px;"></td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Round bottom or three neck flask</td>
			<td style="width:175px;"></td>
			<td style="width:159px;"></td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:297px;">Rubber septums of sufficient size for chosen round bottom or three neck flask</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">5 mL hypodermic syringes</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Hypodermic needles</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Rubber party ballons</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Rubber bands</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="24">
			<td height="24" style="height:24px;width:297px;">A source of N2 gas</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Rotary evaporator</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Drying oven</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">NMR tubes</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">NMR spectrometer</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">500 mL beakers</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Glass or plastic pipettes</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

amide coupling reaction for the synthesis of bispyridine-based ligands and their complexation to platinum as dinuclear anticancer agents

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. Isonicotinic acid, or its derivatives, are coupled to variable length diaminoalkane chains under an inert atmosphere in anhydrous DMF or DMSO with the use of a weak base, triethylamine, and a coupling agent, 1-propylphosphonic anhydride. The products precipitate from solution upon formation or can be precipitated by the addition of water. If desired, the ligands can be further purified by recrystallization from hot water. Dinuclear platinum complex synthesis using the bispyridine ligands is done in hot water using transplatin. The most informative of the chemical characterization techniques to determine the structure and gross purity of both the bispyridine ligands and the final platinum complexes is 1H NMR with particular analysis of the aromatic region of the spectra (7-9 ppm). The platinum complexes have potential application as anticancer agents and the synthesis method can be modified to produce trinuclear and other multinuclear complexes with different hydrogen bonding functionality in the bridging ligand.

비스 피리딘 리간드와 각각 이핵 백금 착체 1 H, 13 C 및 195 편 NMR (표 1 및 2), 및 전기 분무 이온화 질량 분광법에 의해 특징된다. 정확한 융점은 최고의 C, H 및 N 함유율에 대한 원소 분석에 의해 측정되는 시차 주사 열량 및 순도를 사용하여 결정될 수있다. 그것이 결정적 성공 아미드 커플 링과 백금 조정 (표 1, 2)을 입증 할 수 공명과 ?...

Watch this Scientific Journal Video about Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents at JoVE.com

Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents

이 프로토콜은 항암제와 BBR3464 picoplatin의 양태를 결합 다핵 백금 착체의 합성에 사용하기에 적합한 가교 리간드를 형성하기 위해 이소 니코틴산 및 디아 미노 알칸의 아미드 커플 링 반응을 사용하는 방법을 설명한다.

이핵 항암제로 플래티넘 비스 피리딘 계 리간드와 이들 착물의 합성 아미드 커플 링 반응

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. ...

amide-coupling-reaction-for-synthesis-bispyridine-based-ligands-their

Research

JoVE Journal

Chemistry

13.9K 조회수.  The University of Sydney.  이 프로토콜은 항암제와 BBR3464 picoplatin의 양태를 결합 다핵 백금 착체의 합성에 사용하기에 적합한 가교 리간드를 형성하기 위해 이소 니코틴산 및 디아 미노 알칸의 아미드 커플 링 반응을 사용하는 방법을 설명한다. 

비디오: Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents

Anticancer Metal Complexes: Synthesis and Cytotoxicity Evaluation by the MTT Assay

Titanium (IV) and vanadium (V) complexes are highly potent anticancer agents. A challenge in their synthesis refers to their hydrolytic instability; therefore their preparation should be conducted under an inert atmosphere. Evaluation of the anticancer activity of these complexes can be achieved by the MTT assay.
The MTT assay is a colorimetric viability assay based on enzymatic reduction of the MTT molecule to formazan when it is exposed to viable cells. The outcome of the reduction is a color change of the MTT molecule. Absorbance measurements relative to a control determine the percentage of remaining viable cancer cells following their treatment with varying concentrations of a tested compound, which is translated to the compound anticancer activity and its IC50 values. The MTT assay is widely common in cytotoxicity studies due to its accuracy, rapidity, and relative simplicity.
Herein we present a detailed protocol for the synthesis of air sensitive metal based drugs and cell viability measurements, including preparation of the cell plates, incubation of the compounds with the cells, viability measurements using the MTT assay, and determination of IC50 values.

A method for synthesis of air-sensitive titanium and vanadium anticancer agents is described, along with the evaluation of their cytotoxic activity towards human cancer cell line by the MTT Assay.

MTT의 분석에 의해 합성 및 세포 독성 평가 : 항암 금속 합성물

Titanium (IV) and vanadium (V) complexes are highly potent anticancer agents. A challenge in their synthesis refers to their hydrolytic instability; ...

연구

화학

Split-and-pool Synthesis and Characterization of Peptide Tertiary Amide Library

Peptidomimetics are great sources of protein ligands. The oligomeric nature of these compounds enables us to access large synthetic libraries on solid phase by using combinatorial chemistry. One of the most well studied classes of peptidomimetics is peptoids. Peptoids are easy to synthesize and have been shown to be proteolysis-resistant and cell-permeable. Over the past decade, many useful protein ligands have been identified through screening of peptoid libraries. However, most of the ligands identified from peptoid libraries do not display high affinity, with rare exceptions. This may be due, in part, to the lack of chiral centers and conformational constraints in peptoid molecules. Recently, we described a new synthetic route to access peptide tertiary amides (PTAs). PTAs are a superfamily of peptidomimetics that include but are not limited to peptides, peptoids and N-methylated peptides. With side chains on both &#945;-carbon and main chain nitrogen atoms, the conformation of these molecules are greatly constrained by sterical hindrance and allylic 1,3 strain. (Figure 1) Our study suggests that these PTA molecules are highly structured in solution and can be used to identify protein ligands. We believe that these molecules can be a future source of high-affinity protein ligands. Here we describe the synthetic method combining the power of both split-and-pool and sub-monomer strategies to synthesize a sample one-bead one-compound (OBOC) library of PTAs.

Peptide tertiary amides (PTAs) are a superfamily of peptidomimetics that include but are not limited to peptides, peptoids and N-methylated peptides. Here we describe a synthetic method which combines&#160;both split-and-pool and sub-monomer strategies to synthesize a one-bead one-compound library of PTAs.

분할 및 풀 합성 펩타이드 급 아미드 도서관의 특성

Peptidomimetics are great sources of protein ligands. The oligomeric nature of these compounds enables us to access large synthetic libraries on solid ...

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

A protocol for the synthesis and processing of polycrystalline SrTiO3 ceramics doped non-uniformly with Pr is presented along with the investigation of their thermoelectric properties.

불균일 PR-도핑 된 SrTiO3의 합성<sub&gt; 3</sub&gt; 도자기와 그 열전 특성

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma ...

Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

This paper describes the synthesis and peroxide-modification of nanosize monosodium titanate (nMST), along with an ion-exchange reaction to load the material with Au(III) ions. The synthesis method was derived from a sol-gel process used to produce micron-sized monosodium titanate (MST), with several key modifications, including altering reagent concentrations, omitting a particle seed step, and introducing a non-ionic surfactant to facilitate control of particle formation and growth. The resultant nMST material exhibits spherical-shaped particle morphology with a monodisperse distribution of particle diameters in the range from 100 to 150&#160;nm. The nMST material was found to have a Brunauer-Emmett-Teller (BET) surface area of 285 m2g-1, which is more than an order of magnitude higher than the micron-sized MST. The isoelectric point of the nMST measured 3.34 pH units, which is a pH unit lower than that measured for the micron-size MST. The nMST material was found to serve as an effective ion exchanger under weakly acidic conditions for the preparation of an Au(III)-exchange nanotitanate. In addition, the formation of the corresponding peroxotitanate was demonstrated by reaction of the nMST with hydrogen peroxide.

The surfactant mediated sol-gel synthesis of nanosized monosodium titanate is described, along with preparation of the corresponding peroxide modified material. An ion-exchange reaction with Au(III) is also presented.

This paper describes the synthesis and peroxide-modification of nanosize monosodium titanate (nMST), along with an ion-exchange reaction to load the ...

HKUST-1 as a Heterogeneous Catalyst for the Synthesis of Vanillin

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately 200 different odorant compounds in addition to vanillin. The natural extraction of vanillin (from the orchid Vanilla planifolia, Vanilla tahitiensis and Vanilla pompon) represents only 1% of the worldwide production and since this process is expensive and very long, the rest of the production of vanillin is synthesized. Many biotechnological approaches can be used for the synthesis of vanillin from lignin, phenolic stilbenes, isoeugenol, eugenol, guaicol, etc., with the disadvantage of harming the environment since these processes use strong oxidizing agents and toxic solvents. Thus, eco-friendly alternatives on the production of vanillin are very desirable and thus, under current investigation. Porous coordination polymers (PCPs) are a new class of highly crystalline materials that recently have been used for catalysis. HKUST-1 (Cu3(BTC)2(H2O)3, BTC = 1,3,5-benzene-tricarboxylate) is a very well known PCP which has been extensively studied as a heterogeneous catalyst. Here, we report a synthetic strategy for the production of vanillin by the oxidation of trans-ferulic acid using HKUST-1 as a catalyst.

The conversion of trans-ferulic acid to vanillin was achieved by heterogeneous catalysis. HKUST-1 was employed in this synthesis and the essential step in the catalytic process was the generation of unsaturated metal sites. Thus, when the catalyst was activated under vacuum, full vanillin conversion (yield of 95%) was obtained.

HKUST 바닐린-1의 합성에 대해 불균일 촉매로서

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the development of antibody drug conjugates (ADCs) and nanomedicine, fluorescent microscopy and systems chemistry. For many of these applications, specificity of the bioconjugation method used is of prime concern. The Michael addition of maleimides with cysteine(s) on the target proteins is highly selective and proceeds rapidly under mild conditions, making it one of the most popular methods for protein bioconjugation.
We demonstrate here the modification of the only surface-accessible cysteine residue on yeast cytochrome c with a ruthenium(II) bisterpyridine maleimide. The protein bioconjugation is verified by gel electrophoresis and purified by aqueous-based fast protein liquid chromatography in 27% yield of isolated protein material. Structural characterization with MALDI-TOF MS and UV-Vis is then used to verify that the bioconjugation is successful. The protocol shown here is easily applicable to other cysteine - maleimide coupling of proteins to other proteins, dyes, drugs or polymers.

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

This protocol details the important steps required for the bioconjugation of a cysteine containing protein to a maleimide, including reagent purification, reaction conditions, bioconjugate purification and bioconjugate characterization.

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single molecule level. An electrostatic self-assembly and covalent fixation (ESA-CF) process is used for the synthesis of the cyclic poly(tetrahydrofuran) (poly(THF)). The diffusive motion of individual cyclic polymer chains in a melt state is visualized using single molecule fluorescence imaging by incorporating a fluorophore unit in the cyclic chains. The diffusive motion of the chains is quantitatively characterized by means of a combination of mean-squared displacement (MSD) analysis and a cumulative distribution function (CDF) analysis. The cyclic polymer exhibits multiple-mode diffusion which is distinct from its linear counterpart. The results demonstrate that the diffusional heterogeneity of polymers that is often hidden behind ensemble averaging can be revealed by the efficient synthesis of the cyclic polymers using the ESA-CF process and the quantitative analysis of the diffusive motion at the single molecule level using the MSD and CDF analyses.

A protocol for the synthesis and characterization of diffusive motion of cyclic polymers at the single molecule level is presented.

단일 분자 수준에서 순환 고분자의 합성 및 용융 상태에서 그들의 확산 운동의 특성

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single ...

Preparation and In Vitro Characterization of Dendrimer-based Contrast Agents for Magnetic Resonance Imaging

Paramagnetic complexes of gadolinium(III) with acyclic or macrocyclic chelates are the most commonly used contrast agents (CAs) for magnetic resonance imaging (MRI). Their purpose is to enhance the relaxation rate of water protons in tissue, thus increasing the MR image contrast and the specificity of the MRI measurements. Current clinically approved contrast agents are low molecular weight molecules that are rapidly cleared from the body. The use of dendrimers as carriers of paramagnetic chelators can play an important role in the future development of more efficient MRI contrast agents. Specifically, the increase in local concentration of the paramagnetic species results in a higher signal contrast. Furthermore, this CA provides a longer tissue retention time due to its high molecular weight and size. Here, we demonstrate a convenient procedure for the preparation of macromolecular MRI contrast agents based on poly(amidoamine) (PAMAM) dendrimers with monomacrocyclic DOTA-type chelators (DOTA &#8211; 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate). The chelating unit was appended by exploiting the reactivity of the isothiocyanate (NCS) group towards the amine surface groups of the PAMAM dendrimer to form thiourea bridges. Dendrimeric products were purified and analyzed by means of nuclear magnetic resonance spectroscopy, mass spectrometry, and elemental analysis. Finally, high resolution MR images were recorded and the signal contrasts obtained from the prepared dendrimeric and the commercially available monomeric agents were compared.

Preparation and In Vitro Characterization of Dendrimer-based Contrast Agents for Magnetic Resonance Imaging

This protocol describes the preparation and characterization of a dendrimeric magnetic resonance imaging (MRI) contrast agent that carries cyclen-based macrocyclic chelates coordinating paramagnetic gadolinium ions. In a series of MRI experiments in vitro, this agent produced an amplified MRI signal when compared to the commercially available monomeric analogue.

준비 및<em&gt; 체외</em&gt; 자기 공명 영상에 대한 덴드리머 기반 대조 대리인의 특성

Paramagnetic complexes of gadolinium(III) with acyclic or macrocyclic chelates are the most commonly used contrast agents (CAs) for magnetic resonance ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

백 금-니켈 나노 와이어 및 산소 감소 성능 최적화의 합성

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Preparation of Stable Bicyclic Aziridinium Ions and Their Ring-Opening for the Synthesis of Azaheterocycles

Bicyclic aziridinium ions were generated by the removal of an appropriate leaving group through internal nucleophilic attack by nitrogen atom in the aziridine ring. The utility of bicyclic aziridinium ions, specifically 1-azoniabicyclo[3.1.0]hexane and 1-azoniabicyclo[4.1.0]heptane tosylate highlighted in the aziridine ring openings by the nucleophile with the release of the ring strain to yield the corresponding ring-expanded azaheterocycles such as pyrrolidine, piperidine and azepane with diverse substituents on the ring in regio- and stereospecific manner. Herein, we report a simple and convenient method for the preparation of the stable 1-azabicyclo[4.1.0]heptane tosylate followed by selective ring opening via a nucleophilic attack either at the bridge or at the bridgehead carbon to yield piperidine and azepane rings, respectively. This synthetic strategy allowed us to prepare biologically active natural products containing piperidine and azepane motif including sedamine, allosedamine, fagomine and balanol in highly efficient manner.

Bicyclic aziridinium ions such as 1-azoniabicyclo[4.1.0]heptane tosylate were generated from 2-[4-tolenesulfonyloxybutyl]aziridine, which was utilized for the preparation of substituted piperidines and azepanes via regio- and stereospecific ring-expansion with various nucleophiles. This highly efficient protocol allowed us to prepare diverse azaheterocycles including natural products such as fagomine, febrifugine analogue and balanol.

Azaheterocycles의 합성에 대 한 안정적인 Bicyclic Aziridinium 이온과 그들의 반지 개통 준비

Bicyclic aziridinium ions were generated by the removal of an appropriate leaving group through internal nucleophilic attack by nitrogen atom in the ...