资金从欧洲研究委员会收到了欧盟第七框架计划（FP7/2007-2013）下/ ERC赠款协定没有[239603]

<ol><li>步骤2（2.1-2.6），如果一个手套箱不可用，跳到另一种;准备的V（V）配合物（ 图2）; 18行为步骤1.1-1.4的手套箱。 <ol><li>溶解0.42的配位体的毫摩尔的 H 2升的无水THF中，并将其添加到VO的等效量的（O I镨）在THF中的搅拌溶液3。 </li><li>在室温下15分钟搅拌反应混合物，并除去真空下挥发物。 </li><li>加冷正己烷并在真空下将其删除。暗紫色粉末应以定量收率得到。 </li><li>称量得到的化合物的8毫克在Eppendorf管中。跳到第3步。 </li></ol></li><li>使用的Schlenk线制备V（V）络合物。 <ol><li>溶解0.42毫摩尔的配位体H 2升的无水THF中，在干燥的Schlenk烧瓶中，带隔片盖，连接到在Schlenk线，并应用交替真空/惰性气体（N 2或Ar）的环境中，它建议申请3篇UCH轮，等待2-5分钟的真空阶段。 </li><li>用注射器通过隔膜帽加入干燥的THF。 </li><li>加入VO（O I Pr）的同等金额的THF溶液，已被同样准备通过挂钩适当干燥的Schlenk烧瓶中的行，应用惰性环境，并通过从钒解决了的注射器加入试剂3配体。 </li><li>在室温下15分钟搅拌反应混合物，并除去真空下挥发，如果有不稳定的产品的一个问题，进行惰性气氛下挥发的Schlenk型蒸馏;使用惰性气体流，以连接已被预干燥所需的玻璃器皿。 </li><li>加冷正己烷并在真空下将其删除。暗紫色粉末应以定量收率得到。 </li><li>称量得到的化合物的8毫克在Eppendorf管中。 </li></ol></li><li> （Ⅳ）配合物（ 图2）的制备Ti; 28 </s高达&gt;行为的步骤在手套箱3.1-3.3，如果一个手套箱不适，调整为模拟钒（步骤2）雇用的Schlenk行，而不是讨论的替代措施。 <ol><li>溶解0.35的配位体H 2升的无水THF毫摩尔并将其添加到钛（O I Pr）的4在THF中的等量的搅拌溶液中。 </li><li>在室温下2小时搅拌反应混合物。除去真空下挥发物，得到定量产率为黄色产物。 </li><li>称量得到的在Eppendorf小瓶化合物8毫克。 </li></ol></li><li> HT-29细胞的96孔板的下游<ol><li>培养HT-29细胞在75cm 2的烧瓶中，用RPMI-1640培养基中含有1％青霉素/链霉素抗生素，1％L-谷氨酰胺和10％胎牛血清（FBS），在37℃，5％CO 2的。 </li><li>取出介质时，HT-29细胞达到最大汇合（90-100％，每3-4天传代培养无）。用1毫升洗涤胰蛋白酶（0.25％）/ EDTA（0.05％）溶液，并删除它。 </li><li>加入1 ml的胰蛋白酶（0.25％）/ EDTA（0.05％）溶液孵育5分钟。 </li><li>从烧瓶中分离对HT-29细胞加入10毫升培养基中的禁用胰蛋白酶活性。转移5毫升细胞混合物与管。 </li><li>用吸管滴几滴细胞混合物转移到计数器室。计数器室包括5×5格。 </li><li>的4平方在角部和一个在中间：用显微镜计数细胞在5代表正方形。 </li><li>计算细胞目前的估计金额。总结了细胞在5代表正方形和除以20。 </li><li>通过4.7步的结果除以0.6。所接收到的数字是每板所需的细胞混合物的量。该计算是指含有0.6×10 6细胞（每孔9000个细胞）的板。 </li><li>用移液管转移市盈率市所需细胞混合物的量晚期（如计算第4.8节），并添加13.2毫升培养基（每孔×66孔200微升）。 </li><li>由11通道移液器（每孔200微升，6行，66孔总数）的混合物加至96孔板中。每行一个好应为空白对照保持为空。 </li><li>将培养板在37℃，5％CO 2中放置24小时，使细胞附着到板上。 </li></ol></li><li>化合物的插入<ol><li> （根据所期望的浓度范围内，或不同量）的无水THF到各化合物的8毫克加入200μl称量如在步骤1.4（或2.6）或3.3所述。权衡的配位体的 H 2 L 8毫克，也是。 </li><li>在9种不同的Eppendorf小瓶中加入60微升四氢呋喃进一步稀释每个化合物溶液。 </li><li>用移液管加入60μl由5.1节中的混合物在第一的Eppendorf小瓶中，重悬并转移60微升至下一个小瓶中，依此类推，直到传输10个不同的浓度分别为邻btained（包括第5.1父混合物）。 </li><li>稀释20微升各种浓度的THF与180微升培养基。 </li><li>准备一个控制解决方案，用THF仅20微升的THF用180微升培养基中的每个测量。 </li><li>加10微升从所得的溶液（包括十二烷基硫酸钠控制），对每一个已含有200μl的细胞的上述溶液在培养基中以使最终浓度高达200毫克/升的化合物（浓度范围内能很好地根据该化合物的活性）来改变。 </li><li>您可能会发现一些沉淀在根据化合物的溶解度应用的最高浓度。 </li><li>重复该化合物3倍（在相同的化合物的板3行）的各测定，每行包含：用在10个不同的浓度，以及不含有细胞为空白仅用于控制和1与溶剂处理1以及含有细胞的化合物处理过的细胞控制。 </li><li>孵育加载板3天，在37℃下在5％CO 2气氛中。 </li></ol></li><li>采用MTT法测定细胞毒作用<ol><li>通过加入1g MTT粉末到200ml溶液的RPMI-1640培养基中的无酚红制备的MTT溶液。原液可以划分到15ml试管，并存储在-20℃。 </li><li>加入20μl的MTT溶液到每个使用以及11道移液器（除空白对照孔不从步骤4.10的细胞），并孵育板额外的3小时。 </li><li>除去各孔的培养基溶液。 </li><li>添加200μl的异丙醇以每孔以溶解甲。搅动板0.5小时，直到均匀性达到。 </li><li>测量的吸光度在550nm处为200微升通过微量板读数器分光光度计在上述溶液中。 </li><li>各重复测量（包括3次重复，见步骤5.8）在3个不同的日子。 </li><li>计算吨细胞生存力通过从测量值减去空白对照的吸光度值，将结果除以在THF溶剂中的控制值的吸光度，并乘以100％，他的百分比。 </li><li>使用GraphPad Prism软件（或同等学历）计算IC 50值。 </li><li>所报告的IC 50是收集在至少三个不同天所有的IC 50值的平均值，误差值的标准偏差。 </li></ol></li></ol>

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作者宣称他们没有竞争的经济利益。

在这个手稿中描述的方法结合化学合成与生物细胞活力检测。与关于活细胞的任何生物的方法，这是至关重要的，在层流罩的工作，并保持在无菌条件，包括使用无菌有机溶剂。另外，制备的水解不稳定的金属为基础的药物，并存储应进行惰性条件下，对​​其中的手套箱或舒伦克线技术应该被利用。 该技术的选择惰性的环境下工作，主要是依赖于手套箱的可用性。如果有?...

化疗仍然是在临床上用于各种癌症疾病的治疗采用的主要课程之一，并由此研究大量的，目的是开发新的和改进的抗癌药物世界范围内进行。这样的研究大多开始在化学级，与化合物的设计和制备，接着在体外的细胞毒性生物学评价。细胞活力可以通过各种检测，提供对细胞活性1-2的信息进行评估。 顺铂是铂络合物被广泛用作化学治疗药物，它被认为是一种有效的治疗主要针对睾丸癌和卵巢癌3-4的例子。然而，其狭窄的活动范围和严重的副作用引发的其他烈性过渡金属配合物5-8的研究。其中，钛（IV）和钒（V）配合物表现出较高的活性的有希望的结果，并减少毒性9-16。钛（Ⅳ）络合物是第一顺铂后，由于这些特性，进入临床试验，但是，他们并没有审判，由于配方的困难和水解稳定性。因此，有电流需要开发对这些金属配合物可结合高抗癌活性与耐水性15,17-21改进的衍生物。 中的Ti（IV）和V的制备方法的一个挑战（V）配合物是指将前体试剂的水解不稳定性，因此，在惰性气氛应保持。钛（Ⅳ）和V（Ⅴ）化合物的制备方法为N 2或Ar条件下，在手套箱中，或使用的Schlenk线技术下进行。 用于抗癌活性的评价的一个常见方法是基于MTT（3 - （4,5 - dimethylthiazolyl）-2,5 - 二苯基溴化）测定。此法是由Mosmann的提出在1983年比色可行性分析22。它是非常充分的研究和表征，并评估新细胞毒性化合物的效力时，由于其精确度，快速性，及对多种细胞系被应用能力它被认为是高效的。此活力测定是基于当它暴露于活细胞的MTT分子的颜色变化。的吸光度，这是成正比的存活细胞的数量，并且相比于未处理的对照的测定中，使所测试的化合物的细胞生长抑制的能力的评估。 的MTT比色分析法在96孔板形式23进行。该细胞可能需要预培养在添加了测试药物的前孔中。在预温育时间可以从0-24小时，根据细胞系的属性而变化。细胞通常暴露于药物为24-96小时，这取决于药物的活性。 MTT溶液然后被加入到经处理的细胞，其中所述叫喊超重MTT是由多种线粒体和细胞质酶，操作中存活的细胞（ 图1）24减少到紫色的甲（formazan）。将MTT分子不是由死细胞或红细胞（代谢不活跃的细胞），脾细胞（静息细胞）和伴刀豆球蛋白A刺激淋巴细胞（活化细胞）22减小。经过3-4小时培养用MTT甲臜沉淀。甲臜形成0.5小时培养后开始，但为获得最佳结果，最好是将细胞暴露于MTT至少3小时22。因此，在生长介质中被删除，甲溶解在有机溶剂中，优选异丙醇25，虽然DMSO也可以使用26。消除了介质是因为酚红，这是广泛通用于生长培养基中获得准确的结果，并且沉淀的蛋白质可与吸光度测定25干涉的关键。当经残溶液达到均匀，该溶液的吸光度用酶标仪分光光度计测定。在550nm处的吸光度是成正比的细胞以每孔细胞200-50,000的范围内的数目，并且因此可以检测到非常少量的细胞22。的吸光度表示存活细胞是保持与药物治疗后的金额，并进行比较了未暴露于药物的对照细胞的吸光度。通过适当的软件分析的结果提供了IC 50值（抑制浓度50％）的值及其统计误差的基础上，测定重复几次。 MTT分析是广泛通用的细胞毒性研究中用于筛选新的抗癌化合物，由于它的精度和相对简单。然而，使用MTT测定法，它依赖于酶促反应时，必须考虑各种酶抑制剂可以影响一个MTT的还原ð导致错误的结果27。此外，本MTT实验不提供对药物2的细胞毒性活性的分子机理的任何信息。

<table border="1">
	<tbody>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Reagent/Material</td>
		</tr>
		<tr>
			<td>Fetal bovine serum (FBS)</td>
			<td>Biological Industries</td>
			<td>04-007-1A</td>
			<td></td>
		</tr>
		<tr>
			<td>Hexane AR</td>
			<td>Gadot</td>
			<td>830122313</td>
			<td>Dried using a solvent drying system</td>
		</tr>
		<tr>
			<td>HT-29 cell line</td>
			<td>ATCC</td>
			<td>HTB-38</td>
			<td></td>
		</tr>
		<tr>
			<td>Isopropanol AR</td>
			<td>Gadot</td>
			<td>830111370</td>
			<td></td>
		</tr>
		<tr>
			<td>L-glutamine</td>
			<td>Biological Industries</td>
			<td>03-020-1B</td>
			<td></td>
		</tr>
		<tr>
			<td>MTT</td>
			<td>Sigma-Aldrich</td>
			<td>M5655-1G</td>
			<td></td>
		</tr>
		<tr>
			<td>Penicillin/streptomycin antibiotics</td>
			<td>Biological Industries</td>
			<td>03-031-1B</td>
			<td></td>
		</tr>
		<tr>
			<td>RPMI-1640 with phenol red with L-glutamine</td>
			<td>Sigma-Aldrich</td>
			<td>R8758</td>
			<td></td>
		</tr>
		<tr>
			<td>RPMI without phenol red</td>
			<td>Biological Industries</td>
			<td>01-103-1A</td>
			<td></td>
		</tr>
		<tr>
			<td>Tetrahydrofuran (THF) AR</td>
			<td>Gadot</td>
			<td>830156391</td>
			<td>dried using a solvent drying system</td>
		</tr>
		<tr>
			<td>Ti(OiPr)4</td>
			<td>Sigma-Aldrich</td>
			<td>205273-500ML</td>
			<td>moisture sensitive</td>
		</tr>
		<tr>
			<td>Trypsin/EDTA</td>
			<td>Biological Industries</td>
			<td>03-052-1B</td>
			<td></td>
		</tr>
		<tr>
			<td>VO(OiPr)3</td>
			<td>Sigma-Aldrich</td>
			<td>404926-10G</td>
			<td>moisture sensitive</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Equipment</td>
		</tr>
		<tr>
			<td>12-channel pipette 30-300 &#956;l</td>
			<td>Thermo Scientific</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>12-channel pipette 5-50 &#956;l</td>
			<td>Finnpipette</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>75 cm2 flask</td>
			<td>NUNC</td>
			<td>156472</td>
			<td></td>
		</tr>
		<tr>
			<td>96-well plate with lid (flat bottom)</td>
			<td>NUNC</td>
			<td>167008</td>
			<td></td>
		</tr>
		<tr>
			<td>CO2 Incubator</td>
			<td>Binder</td>
			<td>APT.line C150</td>
			<td></td>
		</tr>
		<tr>
			<td>Counter chamber</td>
			<td>Marienfeld-Superior</td>
			<td>650030</td>
			<td></td>
		</tr>
		<tr>
			<td>Eppendorf vial</td>
			<td>KARTELL</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Glove box</td>
			<td>M. Braun</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Laminar flow hood</td>
			<td>ADS LAMINAIRE</td>
			<td>OPTIMALE 12</td>
			<td></td>
		</tr>
		<tr>
			<td>Microplate reader spectrophotometer</td>
			<td>Bio-Tek</td>
			<td>El-800</td>
			<td></td>
		</tr>
		<tr>
			<td>Microscope</td>
			<td>Nikon</td>
			<td>Eclipse TS100</td>
			<td></td>
		</tr>
		<tr>
			<td>Pipette 20-200 &#956;l</td>
			<td>Finnpipette</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Pipette 5-50 &#956;l</td>
			<td>Finnpipette</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

anticancer metal complexes: synthesis and cytotoxicity evaluation by the mtt assay

钛（IV）和钒（V）的配合物是高度有效的抗癌剂。在它们的合成方法的一个挑战是指它们的水解不稳定性，所以它们的制备方法，应在惰性气氛下进行。评价这些复合物的抗癌活性可通过MTT法来实现。 MTT测定是基于酶催还原的MTT分子为甲，当它暴露于活细胞的比色测定法的可行性。减少的结果是在MTT分子的颜色变化。吸光度测量值相对于对照测定下列其与不同浓度的试验化合物，它被转换为所述化合物的抗癌活性，其IC 50值的处理剩余的存活癌细胞的百分比。 MTT法是广泛普遍的，由于其精确性，快速性，和相对简单的细胞毒性研究。 在此，我们预发送一个详细的协议，用于合成气敏感金属类药物和细胞活力的测量，包括制备的细胞板的，该化合物与细胞温育后，使用MTT测定法，并测定IC 50值的可行性测量。

根据既定程序18,28，它们的纯度可以用NMR和元素分析来评估制备的复合物。 从MTT测定接收到的数据进行分析，以评估化合物18,21的细胞毒性。首先，执行从所有其他值减法空白对照吸光度值。第二，在THF溶剂中的控制值被设置为100％生存力，因为没有生长抑制化合物的溶液。根据控制所有其它值被变换成活力的百分比。的浓度应用和计算出的相对存活率百分比...

Watch this Scientific Journal Video about Anticancer Metal Complexes: Synthesis and Cytotoxicity Evaluation by the MTT Assay at JoVE.com

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

一种用于合成气敏感的钛和钒的抗癌剂的方法进行说明，随着朝向通过MTT测定人肿瘤细胞系的细胞毒活性进行评价。

抗癌金属配合物的合成与细胞毒性评价MTT法

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

anticancer-metal-complexes-synthesis-cytotoxicity-evaluation-mtt

Research

JoVE Journal

Chemistry

57.0K 次观看.  The Hebrew University of Jerusalem. 一种用于合成气敏感的钛和钒的抗癌剂的方法进行说明，随着朝向通过MTT测定人肿瘤细胞系的细胞毒活性进行评价。 

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

Structure and Coordination Determination of Peptide-metal Complexes Using 1D and 2D 1H NMR

Copper (I) binding by metallochaperone transport proteins prevents copper oxidation and release of the toxic ions that may participate in harmful redox reactions. The Cu (I) complex of the peptide model of a Cu (I) binding metallochaperone protein, which includes the sequence MTCSGCSRPG (underlined is conserved), was determined in solution under inert conditions by NMR spectroscopy.
NMR is a widely accepted technique for the determination of solution structures of proteins and peptides. Due to difficulty in crystallization to provide single crystals suitable for X-ray crystallography, the NMR technique is extremely valuable, especially as it provides information on the solution state rather than the solid state. Herein we describe all steps that are required for full three-dimensional structure determinations by NMR. The protocol includes sample preparation in an NMR tube, 1D and 2D data collection and processing, peak assignment and integration, molecular mechanics calculations, and structure analysis. Importantly, the analysis was first conducted without any preset metal-ligand bonds, to assure a reliable structure determination in an unbiased manner.

Structure and Coordination Determination of Peptide-metal Complexes Using 1D and 2D 1H NMR

The NMR-solution structure of a metallochaperone model peptide with Cu (I) was determined, and a detailed protocol from sample preparation and 1D and 2D data collection to a three-dimensional structure is described.

Copper (I) binding by metallochaperone transport proteins prevents copper oxidation and release of the toxic ions that may participate in harmful redox ...

科研

化学

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.

This protocol describes the use of amide coupling reactions of isonicotinic acid and diaminoalkanes to form bridging ligands suitable for use in the synthesis of multinuclear platinum complexes, which combine aspects of the anticancer drugs BBR3464 and picoplatin.

酰胺偶联反应为双吡啶基配体及其络合合成，以白金为双核抗癌药物

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

Synthesis and Characterization of Functionalized Metal-organic Frameworks

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy.

Synthesis, activation, and characterization of intentionally designed metal-organic framework materials is challenging, especially when building blocks are incompatible or unwanted polymorphs are thermodynamically favored over desired forms. We describe how applications of solvent-assisted linker exchange, powder X-ray diffraction in capillaries and activation via supercritical CO2 drying, can address some of these challenges.

功能化的合成与表征金属 - 有机骨架

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

Metal-free Synthesis of Ynones from Acyl Chlorides and Potassium Alkynyltrifluoroborate Salts

Ynones are a valuable functional group and building block in organic synthesis. Ynones serve as a precursor to many important organic functional groups and scaffolds. Traditional methods for the preparation of ynones are associated with drawbacks including harsh conditions, multiple purification steps, and the presence of unwanted byproducts. An alternative method for the straightforward preparation of ynones from acyl chlorides and potassium alkynyltrifluoroborate salts is described herein. The adoption of organotrifluoroborate salts as an alternative to organometallic reagents for the formation of new carbon-carbon bonds has a number of advantages. Potassium organotrifluoroborate salts are shelf stable, have good functional group tolerance, low toxicity, and a wide variety are straightforward to prepare. The title reaction proceeds rapidly at ambient temperature in the presence of a Lewis acid without the exclusion of air and moisture. Fair to excellent yields may be obtained via reaction of various aryl and alkyl acid chlorides with alkynyltrifluoroborate salts in the presence of boron trichloride.

The goal of this manuscript is to demonstrate a straightforward method for the preparation of ynones from acyl chloride and potassium alkynyltrifluoroborate salt starting materials. The one-pot reaction proceeds rapidly in the presence of boron trichloride without exclusion of air and moisture.

Ynones从酰氯和钾Alkynyltrifluoroborate盐无金属合成

Ynones are a valuable functional group and building block in organic synthesis. Ynones serve as a precursor to many important organic functional groups ...

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes

Herein we report the synthesis of a tridentate phosphine ligand N(CH2PPh2)3 (N-triphosPh) (1) via a phosphorus based Mannich reaction of the hydroxylmethylene phosphine precursor with ammonia in methanol under a nitrogen atmosphere. The N-triphosPh ligand precipitates from the solution after approximately 1 hr of reflux and can be isolated analytically pure via simple cannula filtration procedure under nitrogen. Reaction of the N-triphosPh ligand with [Ru3(CO)12] under reflux affords a deep red solution that show evolution of CO gas on ligand complexation. Orange crystals of the complex [Ru(CO)2{N(CH2PPh2)3}-&#954;3P] (2) were isolated on cooling to RT. The 31P{1H} NMR spectrum showed a characteristic single peak at lower frequency compared to the free ligand. Reaction of a toluene solution of complex 2 with oxygen resulted in the instantaneous precipitation of the carbonate complex [Ru(CO3)(CO){N(CH2PPh2)3}-&#954;3P] (3) as an air stable orange solid. Subsequent hydrogenation of 3 under 15 bar of hydrogen in a high-pressure reactor gave the dihydride complex [RuH2(CO){N(CH2PPh2)3}-&#954;3P] (4), which was fully characterized by X-ray crystallography and NMR spectroscopy. Complexes 3 and 4 are potentially useful catalyst precursors for a range of hydrogenation reactions, including biomass-derived products such as levulinic acid (LA). Complex 4 was found to cleanly react with LA in the presence of the proton source additive NH4PF6 to give [Ru(CO){N(CH2PPh2)3}-&#954;3P{CH3CO(CH2)2CO2H}-&#954;2O](PF6) (6).

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes

Ruthenium phosphine complexes are widely used for homogeneous catalytic reactions such as hydrogenations. The synthesis of a series of novel tridentate ruthenium complexes bearing the N-triphos ligand N(CH2PPh2)3 is reported. Additionally, the stoichiometric reaction of a dihydride Ru&#8211;N-triphos complex with levulinic acid is described.

一系列钌的合成，表征和反应<em&gt;Ñ</em&gt; -triphos<sup&gt;博士</sup&gt;配合

Herein we report the synthesis of a tridentate phosphine ligand N(CH2PPh2)3 (N-triphosPh) (1) via a phosphorus based Mannich reaction of the ...

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

单金属和双金属前过渡金属碳化物和氮化物纳米粒子的反相微乳液介导的合成

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

Synthesis of a Water-soluble Metal&#8211;Organic Complex Array

We demonstrate a method for the synthesis of a water-soluble multimetallic peptidic array containing a predetermined sequence of metal centers such as Ru(II), Pt(II), and Rh(III). The compound, named as a water-soluble metal-organic complex array (WSMOCA), is obtained through 1) the conventional solution-chemistry-based preparation of the corresponding metal complex monomers having a 9-fluorenylmethyloxycarbonyl (Fmoc)-protected amino acid moiety and 2) their sequential coupling together with other water-soluble organic building units on the surface-functionalized polymeric resin by following the procedures originally developed for the solid-phase synthesis of polypeptides, with proper modifications. Traces of reactions determined by mass spectrometric analysis at the representative coupling steps in stage 2 confirm the selective construction of a predetermined sequence of metal centers along with the peptide backbone. The WSMOCA cleaved from the resin at the end of stage 2 has a certain level of solubility in aqueous media dependent on the pH value and/or salt content, which is useful for the purification of the compound.

Synthesis of a Water-soluble Metal&amp;#8211;Organic Complex Array

A potential general method for the synthesis of water-soluble multimetallic peptidic arrays containing a predetermined sequence of metal centers is presented.

一个水溶性金属 - 有机络合物阵列合成

We demonstrate a method for the synthesis of a water-soluble multimetallic peptidic array containing a predetermined sequence of metal centers such as ...

Palladium N-Heterocyclic Carbene Complexes: Synthesis from Benzimidazolium Salts and Catalytic Activity in Carbon-carbon Bond-forming Reactions

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from benzimidazolium salts. Detailed and generalized protocols are also presented for testing the catalytic activity of such complexes in arylation and Suzuki-Miyaura cross-coupling reactions. Representative results are shown for the catalytic activity of the four complexes in arylation and Suzuki-Miyaura type reactions. For each of the reactions investigated, at least one of the four complexes successfully catalyzed the reaction, qualifying them as promising candidates for catalysis of many carbon-carbon bond-forming reactions. The protocols presented are general enough to be adapted for the synthesis, purification and catalytic activity testing of new palladium N-heterocyclic carbene complexes.

Palladium N-Heterocyclic Carbene Complexes: Synthesis from Benzimidazolium Salts and Catalytic Activity in Carbon-carbon Bond-forming Reactions

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from benzimidazolium salts. The complexes were tested for catalytic activity in arylation and Suzuki-Miyaura reactions. For each reaction investigated, at least one of the four complexes successfully catalyzed the reaction.

钯<em&gt;ñ</em&gt; - 杂环碳烯配合物：苯并咪唑盐的合成和碳 - 碳键合反应中的催化活性

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from ...

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity in aqueous CO2 reduction. Different from traditional metal nanocrystals, the synthesis of metal single atoms involves a matrix material that can confine those single atoms and prevent them from aggregation. We report an electrospinning and thermal annealing method to prepare Ni single atoms dispersed and coordinated in a graphene shell, as active centers for CO2 reduction to CO. During the synthesis, N dopants play a critical role in generating graphene vacancies to trap Ni atoms. Aberration-corrected scanning transmission electron microscopy and three-dimensional atom probe tomography were employed to identify the single Ni atomic sites in graphene vacancies. Detailed setup of electrochemical CO2 reduction apparatus coupled with an on-line gas chromatography is also demonstrated. Compared to metallic Ni, Ni single atom catalyst exhibit dramatically improved CO2 reduction and suppressed H2 evolution side reaction.

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Here, we present a protocol for the synthesis and electrochemical testing of transition metal single atoms coordinated in graphene vacancies as active centers for selective carbon dioxide reduction to carbon monoxide in aqueous solutions.

电化学 CO2还原的过渡金属单原子催化剂的合成及性能表征

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

Synthesis of a Thiol Building Block for the Crystallization of a Semiconducting Gyroidal Metal-sulfur Framework

We present a method for preparing thioester molecules as the masked form of the thiol linkers and their utilization for accessing a semiconducting and porous metal-dithiolene network in the highly ordered single crystalline state. Unlike the highly reactive free-standing thiols, which tend to decompose and complicate the crystallization of metal-thiolate open frameworks, the thioester reacts in situ to provide the thiol species, serving to mitigate the reaction between the mercaptan units and the metal centers, and to improve crystallization consequently. Specifically, the thioester was synthesized in a one-pot procedure: an aromatic bromide (hexabromotriphenylene) reacted with excess sodium thiomethoxide under vigorous conditions to first form the thioether intermediate product. The thioether was then demethylated by the excess thiomethoxide to provide the thiolate anion that was acylated to form the thioester product. The thioester was conveniently purified by standard column chromatography, and then used directly in the framework synthesis, wherein NaOH and ethylenediamine serve to revert in situ the thioester to the thiol linker for assembling the single-crystalline Pb(II)-dithiolene network. Compared with other methods for thiol synthesis (e.g., by cleaving alkyl thioether using sodium metal and liquid ammonia), the thioester synthesis here uses simple conditions and economical reagents. Moreover, the thioester product is stable and can be conveniently handled and stored. More importantly, in contrast to the generic difficulty in accessing crystalline metal-thiolate open frameworks, we demonstrate that using the thioester for in situ formation of the thiol linker greatly improves the crystallinity of the solid-state product. We intend to encourage broader research efforts on the technologically important metal-sulfur frameworks by disclosing the synthetic protocol for the thioester as well as the crystalline framework solid.

Here, we present a one-pot, transition-metal-free synthesis of thiols and thioesters from aromatic halides and sodium thiomethoxide, followed by the preparation of single crystals of a metal-dithiolene network using thiol species generated in situ from the more stable and tractable thioester.

半导体回转金属硫框架结晶的硫醇构建块的合成

We present a method for preparing thioester molecules as the masked form of the thiol linkers and their utilization for accessing a semiconducting and ...