The authors thank the Laboratory Directed Research and Development program at the Savannah River National Laboratory (SRNL) for funding. We thank Dr. Fernando Fondeur for collection and interpretation of the FT-IR spectra and Dr. John Seaman of the Savannah River Ecology Laboratory for the use of the DLS instrument for particle size measurements. We also thank the Dr. Daniel Chan of the University of Washington and the National Institute of Health (Grant #1R01DE021373-01), for funding experiments investigating the ion exchange reactions with Au(III). The Savannah River National Laboratory is operated by Savannah River Nuclear Solutions, LLC for the Department of Energy under contract DE-AC09-08SR22470.

1.纳米钛酸钠的合成（nMST） <ol><li>通过加入0.58毫升25重量％甲醇钠溶液7.62毫升异丙醇，接着1.8毫升异丙醇钛制备的10ml溶液＃1。 </li><li>通过加入0.24毫升超纯水的9.76毫升异丙醇制备的10ml溶液＃2。 </li><li>添加280毫升异丙醇到一个三颈500毫升圆底烧瓶中，接着0.44毫升的Triton X-100的（平均MW 625克/摩尔）。搅拌用磁力搅拌棒将溶液很好。 </li><li>制备双通道注射器泵以0.333毫升/分钟的速率提供解决方案＃1和＃2。 </li><li>负载溶液＃1和＃2到装有管道的长度，将允许从注射泵将溶液输送到下面的500毫升圆底烧瓶中的溶液水平两个单独的10毫升注射器。 </li><li>在搅拌的同时，解＃1和＃2（10每毫升）添加所有使用在步骤1.4中编程的注射泵进行反应。 </li> &lt;利&gt;在加入完成后，盖上烧瓶，并继续在室温搅拌24小时。 </li><li>开盖烧瓶，加热反应混合物至〜82℃（回流的异丙醇）为45-90分钟，随后用氮气吹扫，同时保持加热。异丙醇被蒸发，间歇地添加超纯水，以取代蒸发异丙醇。 </li><li>后大部分异丙醇蒸发并加入水的体积是大约50ml，除去的热量和使反应混合物冷却。 </li><li>通过一0.1微米的尼龙滤纸过滤收集产物，并用水洗涤数次以除去表面活性剂和任何残留的异丙醇。不要过滤干燥。洗涤完成后，从所述过滤器转移浆料进入预称量瓶或小瓶中，并存储作为水​​性浆液。 </li><li>通过确定浆料的固体重量百分比确定产率。这可以通过测量的等分试样的重量进行前和干燥后的淤浆。 </li></ol> 2.金（III）离子交换<ol><li>转移6.50克4.23％（重量）nMST浆液至50毫升离心管中。该量可基于实际重量百分比在上面的步骤1.10所产生的nMST浆料，并且在步骤1.11确定。 </li><li>称出0.0659克氯金酸4·3H 2 O的到1英钱玻璃小瓶。目标的Ti:金质量比为4:1。 </li><li>化解氯金酸4·3H 2 O在约1毫升水，然后转移到含有nMST离心管。冲洗小瓶几次用另外的水，以确保所有的氯金酸4·3H 2 O被转移到含有nMST离心管。 </li><li>稀释用另外的水悬浮液中，必要时，以使总体积至11毫升目标的约15毫米的最终的Au（III）的浓度。 </li><li>包裹离心管箔保持悬浮在黑暗中，一个那么D翻滚振荡器上旋转式烤架的悬浮液为至少4天。 </li><li>通过以3000 xg离心离心15分钟以分离固体收集产物。通过在水中再分散洗固体用蒸馏水洗涤三次，并reisolate通过以3000 xg离心离心15分钟以除去任何未交换金（Ⅲ）。 </li><li>存储最终产物或者作为通过在水中再分散的水悬浮液，或作为通过倾析掉最后的洗涤水和封盖管的湿润固体。存储在黑暗中的产物。 </li></ol> 3. Peroxotitanate的制备<ol><li>转移5克nMST的9.8％（重量）的浆液，以一个小的烧瓶中。 </li><li>称出0.154克30％（重量） 的 H 2 O 2的溶液中。目标的 H 2 O 2 Ti摩尔比为0.25:1。 </li><li>虽然搅拌nMST悬架以及添加0.154克的H 2 O 2溶液滴。当H 2 O 2另外，WHI暂停德固马上变成黄色。 </li><li>在添加完成后搅拌在环境温度下放置24小时进行反应。 </li><li>通过一0.1微米的尼龙过滤器过滤收集产物，并用水洗涤数次以除去任何未反应的 H 2 O 2。不要过滤干燥。洗涤完成后，从所述过滤器转移浆料进入预称量瓶或小瓶中，并存储作为水​​性浆液。 </li></ol>

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The authors have nothing to disclose.

的外来水的存在，例如从不纯试剂，可以改变该反应的结果，从而导致更大或更多分散粒子。因此，应注意，以确保使用干燥的反应物。的异丙醇钛和甲醇钠应储存在干燥器在不使用时。高纯度的异丙醇应也可用于合成。 温度被发现从凝胶起到产品的转化了关键的作用，以颗粒形式。之前和之后加热至82℃显示产物显示为一个半粒状/半凝胶状状态加热之前，但加热产物后出?...

二氧化钛和碱金属钛酸盐在各种应用中广泛使用，例如在涂料和护肤品颜料和作为能量转换和利用光催化剂1-3酸钠钛酸盐已被证明是除去各种阳离子有效的材料在宽范围的通过阳离子交换反应的pH条件4-7 除了刚才所描述的应用中，微米大小的钠钛酸盐和钠peroxotitanates最近已显示也用作治疗金属递送平台。在本申请中，治疗性金属离子如金（Ⅲ），金（Ⅰ），和铂（II）被用于（MST）钛酸酯钠的钠离子与贵金属交换钛酸交换。 在体外试验表明抑制癌症和细菌细胞通过未知的机理的生长。-8,9- 从历史上看，钠钛酸盐已经被烯生产同时使用溶胶-凝胶和导致具有颗粒尺寸范围从几到几百微米的细粉末热液合成技术。4,5,10,11最近，合成方法已被报道，产生纳米二氧化钛，金属-掺杂钛氧化物，和各种各样的其他金属钛酸盐。例子包括钠氧化钛纳米管（NaTONT）或纳米线通过在升高的温度和压力下在过量氢氧化钠的二氧化钛的反应，由过氧钛酸在升高的温度和压力下，15钠过量氢氧化钠的反应12-14钠钛酸纳米纤维和钛酸铯纳米纤维由酸交换的微米大小的钛酸盐的脱层。16 纳米钠钛酸盐和钠peroxotitanates的合成是感兴趣的增强离子交换动力学，它们通常通过膜扩散或颗粒内diffu控制锡永。这些机制是由离子交换剂的颗粒尺寸在很大程度上控制。此外，作为治疗性金属递送平台，钛酸材料的粒度将预期显著影响金属交换的钛酸盐和癌症和细菌细胞之间的相互作用的性质。例如，细菌细胞，这是典型的0.5的量级 - 2微米，可能会与微米大小的颗粒与纳米颗粒的不同的相互作用。此外，非吞噬的真核细胞已被证明为只与一个尺寸小于1微米。17。因此内在化粒子，纳米钠钛酸盐的合成也是感兴趣的便于从钛酸递送平台金属递送和细胞摄取。减少钠钛酸盐和peroxotitanates的尺寸也将增加在金属离子分离的有效容量和提高材料的光化学性质。16,18 &lt;/ SUP&gt;本文介绍了轻度溶胶-凝胶条件下合成纳米钛酸味精（nMST）的协议修改19的nMST相应过氧化物的准备。用离子交换反应加载用Au（III）中的nMST沿也进行了描述。

<table border="0" cellpadding="0" cellspacing="0" width="923">
	<tbody>
		<tr>
			<td>Titanium(IV) isopropoxide</td>
			<td>Sigma Aldrich</td>
			<td>377996</td>
			<td>99.999% trace metals basis</td>
		</tr>
		<tr>
			<td>Isopropyl alcholol, 99.9%</td>
			<td>Sigma Aldrich</td>
			<td>650447</td>
			<td>HPLC grade (Chomasolv)</td>
		</tr>
		<tr>
			<td>Sodium methoxide in methanol</td>
			<td>Sigma Aldrich</td>
			<td>156256</td>
			<td>25 wt%</td>
		</tr>
		<tr>
			<td>Triton X-100</td>
			<td>Sigma Aldrich</td>
			<td>T9284</td>
			<td>BioXtra</td>
		</tr>
		<tr>
			<td>hydrogen tetrachloroaurate(III) trihydrate</td>
			<td>Sigma Aldrich</td>
			<td>G4022</td>
			<td>ACS reagent grade</td>
		</tr>
		<tr>
			<td>hydrogen peroxide (30 wt%)</td>
			<td>Fisher</td>
			<td>H325</td>
			<td>Certified ACS</td>
		</tr>
		<tr>
			<td>10-mL syringes</td>
			<td>Fisher</td>
			<td>14-823-16E</td>
			<td></td>
		</tr>
		<tr>
			<td>Dual channel syringe pump</td>
			<td>Cole Parmer</td>
			<td>EW-74900-10</td>
			<td>Or equivalent programmable dual channel syringe pump</td>
		</tr>
		<tr>
			<td>Tygon tubing 1/8 inch ID, 1/4 inch OD</td>
			<td>Cole Parmer</td>
			<td>EW-0640776</td>
			<td></td>
		</tr>
		<tr>
			<td>Tygon tubing 1/16 inch ID, 1/8 inch OD</td>
			<td>Cole Parmer</td>
			<td>EW-0740771</td>
			<td></td>
		</tr>
		<tr>
			<td>0.1-&#181;m Nylon filter</td>
			<td>Fisher</td>
			<td>R01SP04700</td>
			<td></td>
		</tr>
		<tr>
			<td>Labquake shaker rotisserie</td>
			<td>Thermo Scientific</td>
			<td>4002110Q</td>
			<td></td>
		</tr>
	</tbody>
</table>

synthesis and reaction chemistry of nanosize monosodium titanate

本文描述的合成和钛酸纳米钠的过氧化物改性（nMST），用离子交换反应一起装入用Au（III）离子的材料。合成方法是从用于生产微米级的单钠钛酸（MST），与几个重要的修改，包括改变试剂浓度，省略颗粒种子步骤，和引入非离子表面活性剂，以促进控制溶胶 - 凝胶方法得到的颗粒的形成和生长。所得nMST材料表现出与颗粒直径的范围为100至150纳米的单分散分布球状颗粒形态。该nMST材料被发现具有285 米 2ğ-1，这是比级比微米尺寸的MST高一个数量级以上的布鲁诺尔-埃米特-特勒（BET）表面积。该nMST的等电点测定3.34个pH单位，这是一个pH单位比为微米尺寸的MST测定低。 ŧ他nMST材料被发现作为一个金（Ⅲ）-exchange nanotitanate制备弱酸性的条件下有效的离子交换剂。此外，对应peroxotitanate的形成通过与过氧化氢的nMST的反应证明。

台MST使用溶胶-凝胶方法，其中，四异丙氧基钛（Ⅳ）（TIPT），甲醇钠，和水合并合成并在异丙醇以形成台MST的晶种颗粒的反应。4微米大小的颗粒，然后通过控制加入的额外生长试剂的量。所得颗粒设有无定形芯和具有约10纳米宽的尺寸在长度为50纳米的外部纤维区20 图1A显示了典型的颗粒尺寸分布，如通过动态光散射（DLS），为微米级的MST测量?...

Watch this Scientific Journal Video about Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate at JoVE.com

Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

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.

纳米尺寸钛酸二氢钠的合成和化学反应

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

synthesis-and-reaction-chemistry-of-nanosize-monosodium-titanate

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8.5K 次观看.  Savannah River Consulting, L.L.C.. 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.

视频: Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

Preparation and Use of Samarium Diiodide (SmI2) in Organic Synthesis: The Mechanistic Role of HMPA and Ni(II) Salts in the Samarium Barbier Reaction

Although initially considered an esoteric reagent, SmI2 has become a common tool for synthetic organic chemists. SmI2 is generated through the addition of molecular iodine to samarium metal in THF.1,2-3 It is a mild and selective single electron reductant and its versatility is a result of its ability to initiate a wide range of reductions including C-C bond-forming and cascade or sequential reactions. SmI2 can reduce a variety of functional groups including sulfoxides and sulfones, phosphine oxides, epoxides, alkyl and aryl halides, carbonyls, and conjugated double bonds.2-12 One of the fascinating features of SmI-2-mediated reactions is the ability to manipulate the outcome of reactions through the selective use of cosolvents or additives. In most instances, additives are essential in controlling the rate of reduction and the chemo- or stereoselectivity of reactions.13-14 Additives commonly utilized to fine tune the reactivity of SmI2 can be classified into three major groups: (1) Lewis bases (HMPA, other electron-donor ligands, chelating ethers, etc.), (2) proton sources (alcohols, water etc.), and (3) inorganic additives (Ni(acac)2, FeCl3, etc).3
Understanding the mechanism of SmI2 reactions and the role of the additives enables utilization of the full potential of the reagent in organic synthesis. The Sm-Barbier reaction is chosen to illustrate the synthetic importance and mechanistic role of two common additives: HMPA and Ni(II) in this reaction. The Sm-Barbier reaction is similar to the traditional Grignard reaction with the only difference being that the alkyl halide, carbonyl, and Sm reductant are mixed simultaneously in one pot.1,15 Examples of Sm-mediated Barbier reactions with a range of coupling partners have been reported,1,3,7,10,12 and have been utilized in key steps of the synthesis of large natural products.16,17 Previous studies on the effect of additives on SmI2 reactions have shown that HMPA enhances the reduction potential of SmI2 by coordinating to the samarium metal center, producing a more powerful,13-14,18 sterically encumbered reductant19-21 and in some cases playing an integral role in post electron-transfer steps facilitating subsequent bond-forming events.22 In the Sm-Barbier reaction, HMPA has been shown to additionally activate the alkyl halide by forming a complex in a pre-equilibrium step.23
Ni(II) salts are a catalytic additive used frequently in Sm-mediated transformations.24-27 Though critical for success, the mechanistic role of Ni(II) was not known in these reactions. Recently it has been shown that SmI2 reduces Ni(II) to Ni(0), and the reaction is then carried out through organometallic Ni(0) chemistry.28
These mechanistic studies highlight that although the same Barbier product is obtained, the use of different additives in the SmI2 reaction drastically alters the mechanistic pathway of the reaction. The protocol for running these SmI2-initiated reactions is described.

Preparation and Use of Samarium Diiodide SmI2 in Organic Synthesis: The Mechanistic Role of HMPA and NiII Salts in the Samarium Barbier Reaction

A straightforward procedure for the preparation of samarium diiodide (SmI2) in THF is described. The role of two main additives namely hexamethylphosphoramide (HMPA) and Ni(acac)2 in Sm mediated reactions is demonstrated in the Sm-Barbier reaction.

二碘化钐的制备和使用（SMI<sub&gt; 2</sub&gt;）在有机合成中:HMPA和镍（II）盐的钐巴尔比耶反应的机理作用

Although initially considered an esoteric reagent, SmI2 has become a common tool for synthetic organic chemists. SmI2 is generated through the addition of ...

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 ...

Highly Stereoselective Synthesis of 1,6-Ketoesters Mediated by Ionic Liquids: A Three-component Reaction Enabling Rapid Access to a New Class of Low Molecular Weight Gelators

In organic chemistry ionic liquids (ILs) have emerged as safe and recyclable reaction solvents. In the presence of a base ILs can be deprotonated to form catalytically active N-Heterocyclic Carbenes (NHCs). Here we have used ILs as precatalysts in the addition of &#945;,&#946;-unsaturated aldehydes to chalcones to form 1,6-ketoesters, incorporating an anti-diphenyl moiety in a highly stereoselective fashion. The reaction has a broad substrate scope and several functional groups and heteroaromatics can be integrated into the ketoester backbone in generally good yields with maintained stereoselectivity. The reaction protocol is robust and scalable. The starting materials are inexpensive and the products can be obtained after simple filtration, avoiding solvent-demanding chromatography. Furthermore, the IL can be recycled up to 5 times without any loss of reactivity. Moreover, the 1,6-ketoester end product is a potent gelator in several hydrocarbon based solvents. The method enables rapid access to and evaluation of a new class of low molecular weight gelators (LMWGs) from recyclable and inexpensive starting materials.

Ionic liquids (ILs) mediate fast, simple and cheap access to 1,6-ketoesters in high diastereoselectivities and good yields. The reaction protocol is robust and the 1,6-ketoesters can be obtained in gram scale after a simple filtration protocol. Moreover, the 1,6-ketoesters are potent gelators in hydrocarbon solvents.

1,6-酮酯高立体选择性合成离子液体介导:三组分反应启用快速进入低分子量胶凝剂的新型类

In organic chemistry ionic liquids (ILs) have emerged as safe and recyclable reaction solvents. In the presence of a base ILs can be deprotonated to form ...

Synthesis of Programmable Main-chain Liquid-crystalline Elastomers Using a Two-stage Thiol-acrylate Reaction

This study presents a novel two-stage thiol-acrylate Michael addition-photopolymerization (TAMAP) reaction to prepare main-chain liquid-crystalline elastomers (LCEs) with facile control over network structure and programming of an aligned monodomain. Tailored LCE networks were synthesized using routine mixing of commercially available starting materials and pouring monomer solutions into molds to cure. An initial polydomain LCE network is formed via a self-limiting thiol-acrylate Michael-addition reaction. Strain-to-failure and glass transition behavior were investigated as a function of crosslinking monomer, pentaerythritol tetrakis(3-mercaptopropionate) (PETMP). An example non-stoichiometric system of 15 mol% PETMP thiol groups and an excess of 15 mol% acrylate groups was used to demonstrate the robust nature of the material. The LCE formed an aligned and transparent monodomain when stretched, with a maximum failure strain over 600%. Stretched LCE samples were able to demonstrate both stress-driven thermal actuation when held under a constant bias stress or the shape-memory effect when stretched and unloaded. A permanently programmed monodomain was achieved via a second-stage photopolymerization reaction of the excess acrylate groups when the sample was in the stretched state. LCE samples were photo-cured and programmed at 100%, 200%, 300%, and 400% strain, with all samples demonstrating over 90% shape fixity when unloaded. The magnitude of total stress-free actuation increased from 35% to 115% with increased programming strain. Overall, the two-stage TAMAP methodology is presented as a powerful tool to prepare main-chain LCE systems and explore structure-property-performance relationships in these fascinating stimuli-sensitive materials.

A novel methodology is presented to synthesize and program main-chain liquid-crystalline elastomers using commercially available starting monomers. A wide range of thermomechanical properties was tailored by adjusting the amount of crosslinker, while the actuation performance was dependent on the amount of applied strain during programming.

的可编程主链液晶性弹性体用双级硫醇丙烯酸酯反应合成

This study presents a novel two-stage thiol-acrylate Michael addition-photopolymerization (TAMAP) reaction to prepare main-chain liquid-crystalline ...

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 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.

蛋白质生物缀合物的合成<em&gt;通过</em&gt;半胱氨酸马来酰亚胺化学

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

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and conformality by taking advantage of self-limiting reactions between vapor-phase precursors and the growing film. Perovskite oxides present potential for next-generation electronic materials, but to-date have mostly been deposited by physical methods. This work outlines a method for depositing SrTiO3 (STO) on germanium using ALD. Germanium has higher carrier mobilities than silicon and therefore offers an alternative semiconductor material with faster device operation. This method takes advantage of the instability of germanium's native oxide by using thermal deoxidation to clean and reconstruct the Ge (001) surface to the 2&#215;1 structure. 2-nm thick, amorphous STO is then deposited by ALD. The STO film is annealed under ultra-high vacuum and crystallizes on the reconstructed Ge surface. Reflection high-energy electron diffraction (RHEED) is used during this annealing step to monitor the STO crystallization. The thin, crystalline layer of STO acts as a template for subsequent growth of STO that is crystalline as-grown, as confirmed by RHEED. In situ X-ray photoelectron spectroscopy is used to verify film stoichiometry before and after the annealing step, as well as after subsequent STO growth. This procedure provides framework for additional perovskite oxides to be deposited on semiconductors via chemical methods in addition to the integration of more sophisticated heterostructures already achievable by physical methods.

This work details the procedures for the growth and characterization of crystalline SrTiO3 directly on germanium substrates by atomic layer deposition. The procedure illustrates the ability of an all-chemical growth method to integrate oxides monolithically onto semiconductors for metal-oxide semiconductor devices.

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

Continuous Flow Chemistry: Reaction of Diphenyldiazomethane with p-Nitrobenzoic Acid

Continuous flow technology has been identified as instrumental for its environmental and economic advantages leveraging superior mixing, heat transfer and cost savings through the &#34;scaling out&#34; strategy as opposed to the traditional &#34;scaling up&#34;. Herein, we report the reaction of diphenyldiazomethane with p-nitrobenzoic acid in both batch and flow modes. To effectively transfer the reaction from batch to flow mode, it is essential to first conduct the reaction in batch. As a consequence, the reaction of diphenyldiazomethane was first studied in batch as a function of temperature, reaction time, and concentration to obtain kinetic information and process parameters. The glass flow reactor set-up is described and combines two types of reaction modules with &#34;mixing&#34; and &#34;linear&#34; microstructures. Finally, the reaction of diphenyldiazomethane with p-nitrobenzoic acid was successfully conducted in the flow reactor, with up to 95% conversion of the diphenyldiazomethane in 11 min. This proof of concept reaction aims to provide insight for scientists to consider flow technology&#39;s competitiveness, sustainability, and versatility in their research.

Continuous Flow Chemistry: Reaction of Diphenyldiazomethane with p-Nitrobenzoic Acid

Flow chemistry carries environmental and economic advantages by leveraging superior mixing, heat transfer and cost benefits. Herein, we provide a blueprint to transfer chemical processes from batch to flow mode. The reaction of diphenyldiazomethane (DDM) with p-nitrobenzoic acid, conducted in batch and flow, was chosen for proof of concept.

连续流动化学: Diphenyldiazomethane 与p硝基苯甲酸的反应

Continuous flow technology has been identified as instrumental for its environmental and economic advantages leveraging superior mixing, heat transfer and ...

Synthesis and Mass Spectrometry Analysis of Oligo-peptoids

Peptoids are sequence-controlled peptide-mimicking oligomers consisting of N-alkylated glycine units. Among many potential applications, peptoids have been thought of as a type of molecular information storage. Mass spectrometry analysis has been considered the method of choice for sequencing peptoids. Peptoids can be synthesized via solid phase chemistry using a repeating two-step reaction cycle. Here we present a method to manually synthesize oligo-peptoids and to analyze the sequence of the peptoids using tandem mass spectrometry (MS/MS) techniques. The sample peptoid is a nonamer consisting of alternating N-(2-methyloxyethyl)glycine (Nme) and N-(2-phenylethyl)glycine (Npe), as well as an N-(2-aminoethyl)glycine (Nae) at the N-terminus. The sequence formula of the peptoid is Ac-Nae-(Npe-Nme)4-NH2, where Ac is the acetyl group. The synthesis takes place in a commercially available solid-phase reaction vessel. The rink amide resin is used as the solid support to yield the peptoid with an amide group at the C-terminus. The resulting peptoid product is subjected to sequence analysis using a triple-quadrupole mass spectrometer coupled to an electrospray ionization source. The MS/MS measurement produces a spectrum of fragment ions resulting from the dissociation of charged peptoid. The fragment ions are sorted out based on the values of their mass-to-charge ratio (m/z). The m/z values of the fragment ions are compared against the nominal masses of theoretically predicted fragment ions, according to the scheme of peptoid fragmentation. The analysis generates a fragmentation pattern of the charged peptoid. The fragmentation pattern is correlated to the monomer sequence of the neutral peptoid. In this regard, MS analysis reads out the sequence information of the peptoids.

A protocol is described for the manual synthesis of oligo-peptoids followed by sequence analysis by mass spectrometry.

寡 peptoids 的合成及质谱分析

Peptoids are sequence-controlled peptide-mimicking oligomers consisting of N-alkylated glycine units. Among many potential applications, peptoids have ...

纳米尺寸钛酸二氢钠的合成和化学反应

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二碘化钐的制备和使用（SMI