AP is grateful to Imperial College London for a PhD studentship via the Frankland Chair endowment. Johnson Matthey plc are also thanked for the loan of the precious metal salts used in this work.

注：进行所有合成在通风橱中，只有适当的安全问题已得到确认，并采取措施防止他们之后。个人防护装备，包括实验室外套，手套和护目镜，并应在任何时候都可以穿。 1.合成N，N，N-三（diphenylphosphinomethylene）胺，N（CH 2 PPH 2）3（N- -triphos PH）（1） <ol><li>向200ml的烘箱中干燥经由三个连续真空-氮气循环在双歧管的Schlenk线的Schlenk烧瓶中添加联苯（羟基亚甲基）氯化鏻11（6.99克，24.7毫摩尔），并置于氮气下。 </li><li>添加脱气的甲醇（30ml）和三乙胺（9.5毫升，68.1毫摩尔），并在RT搅拌1小时，以确保转化的鏻盐与hydroxymethene磷化氢。接着，在甲醇中加入脱气的氨水溶液（2M，4.1毫升，8.2毫摩尔）。 </li><li>在回流下2小时加热反应混合物，在此期间，将配体中沉淀出来，为白色固体。 </li><li>虽然N 个 -triphos 博士配位体是对氧化稳定的空气流过的时间很短，以获得最佳的纯度，通过套管26的过滤，除去溶剂在氮气氛下，并用脱气甲醇（3×10毫升）冲洗，得到分析纯的产物，并保存在氮气气氛下。 </li></ol> 2.合成的[Ru（CO）2 {N（CH 2 PPH 2）3}-κ3 P]（2） <ol><li>向200ml的烘箱干燥的Schlenk烧瓶中，在通过三个连续的真空-氮气循环加入正 -Triphos 博士 （1.0克，1.63毫摩尔）和〔茹3（CO）12]（347毫克，0.54毫摩尔），并置于氮气下双岐管的Schlenk线。 </li><li>加入30毫升无水，脱气的甲苯，并把混合物回流12小时。 </li><li>这12个小时的回流后，过滤通过套管将溶液至第二Schlenk烧瓶中，以除去反应过程中形成的少量的金属钌。 </li><li>使用双岐管的Schlenk线配有液氮冷却的捕集器，以诱导复合物的沉淀减少溶剂的体积到大约10毫升真空下。 </li><li>直至完全再溶解发生再结晶的沉淀物，通过加热轻轻（80-90℃）的油浴中，并随后缓慢冷却至RT通过从油浴中取出的热量，但是允许的Schlenk烧瓶中，以保持浸没。离开O / N，得到橙色结晶固体。 </li><li>隔离适于经由上清液到另一炉的套管过滤X射线衍射的橙色结晶干燥的Schlenk烧瓶中。接着，冲洗干燥和脱气的甲苯（2×5毫升）和干燥的真空 O / N的晶体。保存在一个单独的Schlenk烧瓶中的合并的上清液和洗液。 </li><li>从合并的上清液和漂洗溶液得到第二批晶体S按类似的再结晶过程中的步骤2.5和2.6，以提高反应的总产率。 </li><li>储存在氮气氛下的复杂的暴露于空气中会导致缓慢转化为氧化碳酸盐复合物（见下文）。 </li></ol> 3.合成的[Ru（CO 3）（CO）{N（CH 2 PPH 2）3}-κ3 P]（3） <ol><li>到200毫升的Schlenk烧瓶中，加入2（280毫克，0.364毫摩尔）和5毫升甲苯，以产生部分溶解的橙色悬浮液。 </li><li>插入连接于氧气进入悬浮液和气泡的氧气的气球的针在通过反应混合物持续10分钟的速率为每秒2-3气泡。 </li><li>为橙色沉淀物，通过过滤在空气中收集，并用甲苯（2×5ml）和乙醚（2×5毫升），并真空干燥，得到一种自由流动的橙色粉末，这是在空气中稳定。 </li><li>为了生长适合X-射线DIFFR晶体动作，通过缓慢地使该溶剂耗尽小瓶的侧溶解的3 100毫克的3ml二氯甲烷在顶部的小瓶和层3毫升甲苯。 <ol><li>离开这个O / N，得到结晶。通过倾析上清液，并洗涤该甲苯（2×3毫升）和乙醚（2×3毫升）隔离晶体。燥，真空在双歧管的Schlenk线。 </li></ol></li></ol> 4.合成的[Ru（H）2（CO）{N（CH 2 PPH 2）3}-κ3 P]（4） <ol><li>制备的3（763毫克，0.953毫摩尔）于20毫升无水的溶液，脱气THF中并在氮气正压（0.2巴）注入100ml高压釜工程师的高压反应器中。 </li><li>在反应器顶部空间气体改变为100％的氢气和加压到15巴，在室温，然后加热至100℃并搅拌2小时。 注意！确保所有安全程序已经坚持采用高时，压力系统！ </li><li>冷却至RT后，小心地排出过量的氢气在反应器液面上空间变为氮。 </li><li>将反应溶液转移至氮气下的100毫升的Schlenk烧瓶，并重新连接到双歧管的Schlenk线，滤波器通过套管后和稀释用20毫升无水，脱气甲醇。 </li><li>根据使用双岐管的Schlenk线装有一个液氮真空除去溶剂冷却阱，得到橙色粉末。用无水，脱气的甲醇（3×5毫升）和干燥的洗涤此橙色粉末，脱气乙醚（3×5毫升）和干燥的真空。 </li><li>生长适合X-射线衍射分析的晶体直径：/ N从4分层与无水的等体积量的饱和无水并脱气的甲苯溶液，脱气甲醇。 </li><li>储存在氮气氛下的复合物。 </li></ol> 5.反应〔期RuH 2（CO）{N（CH 2 PPH 2）3}-κ3 P]（4）用NH 4 PF 6和乙酰丙酸<ol><li>制备4在2ml无水的溶液（48.4毫克，65.2微摩尔），脱气的甲苯在炉中干燥的Schlenk烧瓶中，然后通过注射器添加的NH 4 PF 6的搅拌的溶液（10.6毫克，65.0微摩尔）在乙腈（2毫升）在一个单独的炉中干燥的Schlenk烧瓶中。 </li><li>在RT搅拌反应混合物2小时。之后，使用双岐管的Schlenk线配有液氮冷却的捕集器，得到中间体络合物[期RuH（CO）（MeCN中）{N（CH 2 PPH 2）3}-κ3 P]（除去溶剂，真空 5）。 </li><li>用干洗净，脱气己烷（3×3毫升）和干燥的真空分离络合物5，为棕色粉末。 </li><li>到的5在0.5ml中的溶液脱气丙酮-d 6，在0.5ml脱气丙酮-d 6的添加乙酰丙酸（10.8毫克，93.0微摩尔，1.43当量）。用2分钟搅拌反应混合物旋涡搅拌器。 </li><li>记录1 H和30 P {1 1 H}反应每小时16小时，观察反应NMR谱。27 </li></ol>

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The authors have nothing to disclose.

这里我们描述了高效的合成方法对于三齿膦配位体的合成和一系列钌配合物。 N 个 -triphos 博士配位体（1）可以高产率与一个简约的处理过程容易地制备。用于合成这些类型的配体的本磷基曼尼希反应是相当普遍的，并可以用于其它配位体的衍生物具有不同R基团上的P原子。10-12,15-18此外，这种合成方法是适合于在类似的碳为中心的三磷酸配位体，并且可以使用?...

钌膦基配合物是一些最广泛的研究和化学多功能分子催化剂。1-9典型地，这种钌催化剂包含决定了复杂的电子，空间相互作用，几何形状和溶解性或者单-或二齿配位体，并且其深刻地影响到催化活性。多齿膦系统已被广泛地少研究了催化，因为它们是公知的，由于多个磷供体在金属中心越大螯合效果与金属中心赋予更大的稳定性。这样的稳定​​可以是不希望的催化，然而，在更苛刻的反应条件下（较高的温度和压力下）这样的配体的配合物稳定性质可以是在确保催化剂完整性是有利的。我们10-12和13-18人已经调查传授复杂的稳定性和面部 COOR一个这样的多齿膦配体系统dination几何就是所谓 N- -triphos配体系列，其中3膦臂附着到心尖桥接氮原子形成一个潜在的三齿配体。其中一个主要的功能，以这些特定的配位体是容易的方式，它们可通过基于磷从容易得到的仲膦曼尼希反应（ 图1）来合成，因此，膦与各种R基团的，可以以高产率通常制备并以最少的工作了。这一方法的总的目标是提出一个浅显路线通过该钌配合物二氢化设有Ñ-triphos配体可用于随后的催化应用程序进行访问。最近，钌三磷酸基配合物已经引起注意，因为催化剂的衍生自生物质的产品，如乙酰丙酸，19,20生物酯11,21和二氧化碳22至更高的值的化学物质的氢化反应。将是有利展开属于任一，或比已报道，特别是如果它们是合成更容易访问，例如作为 N -triphos配位体的系统的更多活性钌三磷酸衍生物的范围。研究最多的碳为中心的模拟通常患有低产合成并涉及高度空气敏感金属磷化物的试剂，不同于N 个 -triphos配位体，这是更适应，更容易制备。10-18 Ñ-triphos配体保持相对不足的调查，只有钼，钨，钌，铑和金的复合物已报道从9出版物。与此形成鲜明对比的是硼碳为中心的类似物，为此，每年大约有50 900篇，分别以独特的化合物的大量。在亲手性烯烃23，我们在不对称催化加氢尽管如此，含有复合ñ-triphos发现应用程序LL的N作为不对称cyclohydroamination -protectedγ-丙二烯基磺酰胺。24此外，钌络合物由笨重Ñ-triphos配体具有磷杂配位部分的协调被认为激活硅烷，在有机硅化学的发展的关键步骤。25 由于在催化正在进行的研究项目的一部分，我们试图准备了一系列钌ñ-triphos 博士预催化剂，并研究它们的化学计量反应和催化潜力。尽管N 个 -triphos 博士最早被报道在25年前钼复合物，它们的应用，催化或以其他方式还没有被查处。这项工作表明N 个 -triphos支架，这尽管是普遍欠发达，拥有许多理想的特性，如复杂的稳定应用。在这里我们报告的合成路线和表征一系列钌Ñ-triphos 博士络合物可能会发现在催化氢化反应中的应用。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Methanol</td>
			<td rowspan="5">&#8211;</td>
			<td rowspan="5">&#8211;</td>
			<td rowspan="5">Obtained from in-house solvent purification system: Innovative Technology, inc &#34;pure solv&#34; drying tower. Stored in ampules over activated molecular sieves under nitrogen.</td>
		</tr>
		<tr>
			<td>Toluene</td>
		</tr>
		<tr>
			<td>Diethyl Ether</td>
		</tr>
		<tr>
			<td>Tetrahydrofuran (THF)</td>
		</tr>
		<tr>
			<td>Acetonitrile</td>
		</tr>
		<tr>
			<td>d6-Acetone</td>
			<td>VWR</td>
			<td>VWRC87152.0011</td>
			<td>Store in fridge</td>
		</tr>
		<tr>
			<td>Triethylamine</td>
			<td>Sigma-Aldrich</td>
			<td>TO886-1L</td>
			<td>Distilled and stored over activated molecular sieves under N2</td>
		</tr>
		<tr>
			<td>2M Ammonia solution in methanol</td>
			<td>Sigma-Aldrich</td>
			<td>341428-100ML</td>
			<td>Solution comes in a &#34;Sure-Seal&#34; bottle</td>
		</tr>
		<tr>
			<td>NH4PF6</td>
			<td>Sigma-Aldrich</td>
			<td>216593-5G</td>
			<td>Store in desiccator</td>
		</tr>
		<tr>
			<td>Levulinic Acid</td>
			<td>Acros Organics</td>
			<td>125142500</td>
			<td>Solid but melts close to room temperature</td>
		</tr>
		<tr>
			<td>3 &#197; Molecular sieves</td>
			<td>Alfa Aesar</td>
			<td>LO5359</td>
			<td>Activate by heating over night under vacuum</td>
		</tr>
		<tr>
			<td>Schlenk flasks</td>
			<td>GPE</td>
			<td>Custom design</td>
			<td>&#8211;</td>
		</tr>
		<tr>
			<td>Dual-manifold Schlenk line</td>
			<td>GPE</td>
			<td>Custom design</td>
			<td>Dual-manifold of i) N2 that has been passed through a silica drying column and ii) vacuum.</td>
		</tr>
		<tr>
			<td>Rotary vacuum pump</td>
			<td>Edwards</td>
			<td>RV3 A652-01-903</td>
			<td>&#8211;</td>
		</tr>
		<tr>
			<td>100 ml Autoclave Engineer&#39;s high pressure reactor</td>
			<td>Autoclave Engineer</td>
			<td>Custon design</td>
			<td>&#8211;</td>
		</tr>
		<tr>
			<td>Vortex Stirrer</td>
			<td>VWR</td>
			<td>444-1378</td>
			<td>&#8211;</td>
		</tr>
	</tbody>
</table>

the synthesis, characterization and reactivity of a series of ruthenium n-triphosph complexes

这里我们通过hydroxylmethylene膦前体与氨在氮气气氛下的磷基曼尼希反应在甲醇中报告一个三齿膦配位体N（CH 2 PPH 2）3（N- -triphos PH）（1）的合成。 N 个 -triphos 博士配体沉淀从溶液后约1小时回流，并可以分离，通过简单的过滤套管程序下，氮分析纯。在回流下N 个 -triphos 博士配体的[Ru 3（CO）12]的反应得到，显示CO气体对配体络合进化深红色溶液。复杂的[Ru（CO）2 {N（CH 2 PPH 2）3}-κ3 P]（2）中被隔绝在冷却至RT的橙色结晶。 31 P {1 1 H} NMR谱表明的特征单峰在较低频率相比于游离配体。的配合物2的甲苯溶液与氧气反应导致的碳酸盐配合物的[Ru（CO 3）（CO）{N（CH 2 PPH 2）3}-κ3 P〕瞬时沉淀（3），为空气稳定橙色固体。 3在15巴氢气在高压反应器中随后的氢化，得到二氢化物[期RuH 2（CO）{N（CH 2 PPH 2）3}-κ3 P]（4），将其充分利用X射线晶体学和核磁共振光谱。配合物3和4是潜在为一系列氢化反应，包括生物质衍生的产品，如乙酰丙酸（LA）的有用催化剂前体。配合物4被发现与干净的LA反应在质子源添加剂的存在的NH 4 PF 6，得到的[Ru（CO）{N（CH 2 PPH 2）3}-κ3 P {CH 3 CO（CH 2）2 CO 2 H}-κ2 O]（PF 6）（6）。

N个 -triphos 博士配位体（1）和钌配合物系列：钌（CO）2 {N（CH 2 PPH 2）3}-κ3 P]（2）中 ，使用[Ru（CO 3）（CO）{N （CH 2 PPH 2）3}-κ3 P]（3）和使用[Ru（H）2（CO）{N（CH 2 PPH 2）3}-κ3 P]（4）通过1 H组特征， 13 C <s...

Watch this Scientific Journal Video about The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes at JoVE.com

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

钌膦配合物被广泛地用于均相催化反应，例如氢化反应。的一系列新的三齿钌配合轴承N个 -triphos配位体N（CH 2 PPH 2）3的合成的报道。另外，一个二氢化汝Ñ-triphos络合物与乙酰丙酸的化学计量反应进行说明。

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 ...

the-synthesis-characterization-reactivity-series-ruthenium-n

Research

JoVE Journal

Chemistry

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

12.0K 次观看.  Imperial College London. 钌膦配合物被广泛地用于均相催化反应，例如氢化反应。的一系列新的三齿钌配合轴承N个 -triphos配位体N（CH 2 PPH 2）3的合成的报道。另外，一个二氢化汝Ñ-triphos络合物与乙酰丙酸的化学计量反应进行说明。 

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

Production of Disulfide-stabilized Transmembrane Peptide Complexes for Structural Studies

Physical interactions among the lipid-embedded alpha-helical domains of membrane proteins play a crucial role in folding and assembly of membrane protein complexes and in dynamic processes such as transmembrane (TM) signaling and regulation of cell-surface protein levels. Understanding the structural features driving the association of particular sequences requires sophisticated biophysical and biochemical analyses of TM peptide complexes. However, the extreme hydrophobicity of TM domains makes them very difficult to manipulate using standard peptide chemistry techniques, and production of suitable study material often proves prohibitively challenging. Identifying conditions under which peptides can adopt stable helical conformations and form complexes spontaneously adds a further level of difficulty. Here we present a procedure for the production of homo- or hetero-dimeric TM peptide complexes from materials that are expressed in E. coli, thus allowing incorporation of stable isotope labels for nuclear magnetic resonance (NMR) or non-natural amino acids for other applications relatively inexpensively. The key innovation in this method is that TM complexes are produced and purified as covalently associated (disulfide-crosslinked) assemblies that can form stable, stoichiometric and homogeneous structures when reconstituted into detergent, lipid or other membrane-mimetic materials. We also present carefully optimized procedures for expression and purification that are equally applicable whether producing single TM domains or crosslinked complexes and provide advice for adapting these methods to new TM sequences.

Biophysical and biochemical studies of interactions among membrane-embedded protein domains face many technical challenges, the first of which is obtaining appropriate study material. This article describes a protocol for producing and purifying disulfide-stabilized transmembrane peptide complexes that are suitable for structural analysis by solution nuclear magnetic resonance (NMR) and other analytical applications.

生产二硫键稳定的跨膜肽复合物的结构研究

Physical  interactions among the lipid-embedded alpha-helical domains of membrane  proteins play a crucial role in folding and assembly of membrane ...

科研

化学

Isolation and Chemical Characterization of Lipid A from Gram-negative Bacteria

Lipopolysaccharide (LPS) is the major cell surface molecule of gram-negative bacteria, deposited on the outer leaflet of the outer membrane bilayer. LPS can be subdivided into three domains: the distal O-polysaccharide, a core oligosaccharide, and the lipid A domain consisting of a lipid A molecular species and 3-deoxy-D-manno-oct-2-ulosonic acid residues (Kdo). The lipid A domain is the only component essential for bacterial cell survival. Following its synthesis, lipid A is chemically modified in response to environmental stresses such as pH or temperature, to promote resistance to antibiotic compounds, and to evade recognition by mediators of the host innate immune response. The following protocol details the small- and large-scale isolation of lipid A from gram-negative bacteria. Isolated material is then chemically characterized by thin layer chromatography (TLC) or mass-spectrometry (MS). In addition to matrix-assisted laser desorption/ionization-time of flight (MALDI-TOF) MS, we also describe tandem MS protocols for analyzing lipid A molecular species using electrospray ionization (ESI) coupled to collision induced dissociation (CID) and newly employed ultraviolet photodissociation (UVPD) methods. Our MS protocols allow for unequivocal determination of chemical structure, paramount to characterization of lipid A molecules that contain unique or novel chemical modifications. We also describe the radioisotopic labeling, and subsequent isolation, of lipid A from bacterial cells for analysis by TLC. Relative to MS-based protocols, TLC provides a more economical and rapid characterization method, but cannot be used to unambiguously assign lipid A chemical structures without the use of standards of known chemical structure. Over the last two decades isolation and characterization of lipid A has led to numerous exciting discoveries that have improved our understanding of the physiology of gram-negative bacteria, mechanisms of antibiotic resistance, the human innate immune response, and have provided many new targets in the development of antibacterial compounds.

Isolation and characterization of the lipid A domain of lipopolysaccharide (LPS) from gram-negative bacteria provides insight into cell surface based mechanisms of antibiotic resistance, bacterial survival and fitness, and how chemically diverse lipid A molecular species differentially modulate host innate immune responses.

隔离和脂质A的化学表征革兰氏阴性菌

Lipopolysaccharide (LPS) is the major cell surface molecule of gram-negative bacteria, deposited on the outer leaflet of the outer membrane bilayer. LPS ...

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.

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; ...

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.

分裂和池合成及肽叔酰胺图书馆表征

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

Nucleoside Triphosphates - From Synthesis to Biochemical Characterization

The traditional strategy for the introduction of chemical functionalities is the use of solid-phase synthesis by appending suitably modified phosphoramidite precursors to the nascent chain. However, the conditions used during the synthesis and the restriction to rather short sequences hamper the applicability of this methodology. On the other hand, modified nucleoside triphosphates are activated building blocks that have been employed for the mild introduction of numerous functional groups into nucleic acids, a strategy that paves the way for the use of modified nucleic acids in a wide-ranging palette of practical applications such as functional tagging and generation of ribozymes and DNAzymes. One of the major challenges resides in the intricacy of the methodology leading to the isolation and characterization of these nucleoside analogues.
	
	In this video article, we present a detailed protocol for the synthesis of these modified analogues using phosphorous(III)-based reagents. In addition, the procedure for their biochemical characterization is divulged, with a special emphasis on primer extension reactions and TdT tailing polymerization. This detailed protocol will be of use for the crafting of modified dNTPs and their further use in chemical biology.

The protocol described herein aims to explain and abridge the numerous obstacles in the way of the intricate route leading to modified nucleoside triphosphates. Consequently, this protocol facilitates both the synthesis of these activated building-blocks and their availability for practical applications.

核苷三磷酸 - 从合成到生化特征

The  traditional strategy for the introduction of chemical functionalities is the  use of solid-phase synthesis by appending suitably modified ...

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 ...

Synthesis and Characterization of Supramolecular Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

超分子胶体的合成与表征

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

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.

环状聚合物的合成及其在熔融状态扩散运动的表征在单分子水平

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 ...

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of Chalcogenidoplumbates(II or IV)

The phases of &#34;PbCh2&#34; (Ch = Se, Te) are obtained from solid-state syntheses (i.e., by the fusion of the elements under inert conditions in silica glass ampules). Reduction of such phases by elemental alkaline metals in amines affords crystalline chalcogenidoplumbate(II) salts comprised of [PbTe3]2- or [Pb2Ch3]2- anions, depending upon which sequestering agent for the cations is present: crown ethers, like 18-crown-6, or cryptands, like [2.2.2]crypt. Reactions of solutions of such anions with transition-metal compounds yield (poly-)chalcogenide anions or transition-metal chalcogenide clusters, including one with a &#181;-PbSe ligand (i.e., the heaviest-known CO homolog).
In contrast, the solid-state synthesis of a phase of the nominal composition &#34;K2PbSe2&#34; by successive reactions of the elements and by the subsequent solvothermal treatment in amines yields the first non-oxide/halide inorganic lead(IV) compound: a salt of the ortho-selenidoplumbate(IV) anion [PbSe4]4-. This was unexpected due to the redox potentials of Pb(IV) and Se(-II). Such methods can further be applied to other elemental combinations, leading to the formation of solutions with binary [HgTe2]2- or [BiSe3]3- anions, or to large-scale syntheses of K2Hg2Se3 or K3BiSe3 via the solid-state route.
All compounds are characterized by single-crystal X-ray diffraction and elemental analysis; solutions of plumbate salts can be investigated by 205Pb and 77Se or 127Te NMR techniques. Quantum chemical calculations using density functional theory methods enable energy comparisons. They further allow for insights into the electronic configuration and thus, the bonding situation. Molecular Rh-containing Chevrel-type compounds were found to exhibit delocalized mixed valence, whereas similar telluridopalladate anions are electron-precise; the cluster with the &#181;-PbSe ligand is energetically favored over a hypothetical CO analog, in line with the unsuccessful attempt at its synthesis. The stability of formal Pb(IV) within the [PbSe4]4- anion is mainly due to a suitable stabilization within the crystal lattice.

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of ChalcogenidoplumbatesII or IV

The synthesis of chalcogenidoplumbates(II,IV) via the in situ reduction of nominal "PbCh2" (Ch = Chalcogen) and via a solid-state reaction and subsequent solvothermal reactions is presented. Additionally, reactivities of plumbate(II) solutions are portrayed, which yield the heaviest-known CO homolog known to date: the &#181;-PbSe ligand.

结合固态和基于解决方案的技术合成及Chalcogenidoplumbates的反应（II或IV）

The phases of &#34;PbCh2&#34; (Ch = Se, Te) are obtained from solid-state syntheses (i.e., by the fusion of the elements under inert conditions in silica ...

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 ...