この作品は、国家自然科学基金、中国の (21502023) によって支えられました。

1. 合成の 1-(Iodoethynyl)-4-メチル ベンゼン類 (2, 1-Iodoalkynes)
<ol><li>TBAI と CH3CN 3 mL の磁気撹拌棒、空気に開いているを含む反応管に 133 mg (0.36 mmol) を追加します。その後、38 μL を追加 (0.3 mmol) 変らずを使用して混合物にptolylethyne の。</li>
	<li>PIDA のへらを使用して 20 分の期間にわたっての 10 部分で積極的に撹拌した反応混合物に 96.6 mg (0.3 mmol) を追加します。</li>
	<li>3 時間室温で反応混合物をかき混ぜなさい。</li>
	<li>得られた混合物を注ぎ、水の 30 mL が含まれています, 漏斗と水性 Na2S2O3 (10%、0.5 mL) を癒します。酢酸エチル 10 mL で 3 回水の層を抽出します。</li>
	<li>無水硫酸ナトリウム (0.5 g) を 10 ml の飽和食塩水と乾燥した有機層を洗ってください。</li>
	<li>ブフナーを使用して硫酸ナトリウムを離れてしみ出る、粗生成物を得るために減らされた圧力の下で濾液を集中します。</li>
	<li>溶離液にヘキサンを用いたシリカゲル カラムクロマトグラフィーにより粗製品を浄化します。純粋な製品で、1-(iodoethynyl)-4-メチル ベンゼン類が (71.9 mg, 99% の利回り; 淡黄色の液体として得られるRf= 0.79)。</li>
	<li>1H と13C の NMR 分光法および高速液体クロマトグラフィー (HPLC) による製品を分析します。</li>
</ol>2.-1 (E) の合成-(1,2-Diiodovinyl) 4 メチル ベンゼン類 (3, 1, 2-Diiodoalkenes)
<ol><li>磁気撹拌棒、空気に開いているを含む反応管に氣と CH3CN の 1 mL 124.5 mg (0.75 mmol) を追加します。変らずを介して混合物にptolylethyne と H2O 3 mL の 38 μ L (0.3 mmol) を追加します。</li>
	<li>PIDA のへらを使用して 20 分の期間にわたっての 10 部分で積極的に撹拌した反応混合物に 96.6 mg (0.3 mmol) を追加します。</li>
	<li>24 時間室温で反応混合物をかき混ぜなさい。</li>
	<li>得られた混合物を注ぐ水の 30 mL が含まれています, 漏斗、水性 Na2S2O3 (10%、1 mL)、消すし、酢酸エチル 10 mL で 3 回水の層を抽出します。</li>
	<li>食塩水 10 mL でした有機層を洗浄し、無水硫酸ナトリウム (0.5 g) 上乾燥します。</li>
	<li>ブフナーを使用して硫酸ナトリウムを離れてしみ出る、粗生成物を得るために減らされた圧力の下で濾液を集中します。</li>
	<li>溶離液としてヘキサンを用いたシリカゲル カラムクロマトグラフィーにより粗製品を浄化します。純粋なプロダクト、(E)-1 (111.9 mg, 収率 98%; 淡黄色の液体として得られる-(1,2-diiodovinyl)-4-メチル ベンゼン類、Rf = 0.84)。</li>
	<li>1H、 13C の NMR 分光法、高速液体クロマトグラフィーによる製品を分析します。</li>
</ol>3. 合成 1-メチル - 4-(1,2,2-Triiodovinyl) ベンゼン (4, 1,1,2-Triiodoalkenes)
<ol><li>TBAI と CH3CN の 1 mL の空気に開いている撹拌棒を含む反応管に 133 mg (0.36 mmol) を追加します。Ptolylethyne 変らずを使用しての 38 μ L (0.3 mmol) を追加します。</li>
	<li>PIDA のへらを使用して 20 分の期間にわたっての 10 部分で積極的に撹拌した反応混合物に 96.6 mg (0.3 mmol) を追加します。3 h の反応混合物を室温で攪拌します。</li>
	<li>反応混合物に氣の H2O 3 ml 124.5 mg (0.75 mmol) を追加します。</li>
	<li>ヘラを使用して 20 分の期間にわたって PIDA の 193.2 mg (0.6 モル) を 10 の部分で反応混合物に追加します。室温でさらに 3 時間反応混合物をかき混ぜなさい。</li>
	<li>反応混合物に氣の H2O 3 mL、1 mL の CH3CN 別 124.5 mg (0.75 mmol) を追加します。</li>
	<li>PIDA のへらを使用して 20 分の期間にわたっての 10 の部分で反応混合物に別 193.2 mg (0.6 モル) を追加します。別の 12 h の反応混合物を室温で攪拌します。</li>
	<li>得られた混合物を注ぐ水の 30 mL が含まれています, 漏斗、水性 Na2S2O3 (10%、2 mL)、消すし、酢酸エチル 10 mL で 3 回水の層を抽出します。</li>
	<li>食塩水 10 mL でした有機層を洗浄し、無水硫酸ナトリウム (0.5 g) 上乾燥します。</li>
	<li>ブフナーを使用して硫酸ナトリウムを離れてしみ出る、粗生成物を得るために減らされた圧力の下で濾液を集中します。</li>
	<li>1 純粋な製品を得るためにヘキサンを用いたシリカゲル カラムクロマトグラフィーにより粗製品を浄化-メチル - 4-(1, 2, 2-triiodovinyl) ベンゼン、(138.4 mg、93% の利回り; 黄色の液体としてRf = 0.79)。</li>
	<li>1H、 13C の NMR 分光法、高速液体クロマトグラフィーによる製品を分析します。</li>
</ol>4. モノラル、ディ、または高速液体クロマトグラフィーによる末端アルキンのトライ ヨウ素に対する選択度の定量
注: モノラル、ディ、トリ-チログロブリン、アルキン選択性は高速液体クロマトグラフィーによって決定されました。5 μm、4.6 mm × 150 mm のコラム、CH3CN/H2O を使用して計測器を高速液体クロマトグラフィーを行った溶媒, 1.0 mL/min の流量検出器波長λと 75/25 (v/v) を = = 254 nm。
<ol><li>高速液体クロマトグラフィーのための外部の標準溶液の調製<ol>
<li>2を正確に量り (1-(iodoethynyl)-4-ベンゼン; 9.58 mg、39.58 × 10-3モル)、 3 ((E)-1-(1,2-diiodovinyl) 4 ベンゼン; 19.29 mg、52.14 × 10-3モル)、および4 (1-メチル - 4-(1,2,2-triiodovinyl) ベンゼン;11.10 mg、22.38 × 10-3モル)。</li>
		<li>ミックスし CH3CN の 1 mL にこれらの 3 つの化合物を溶解し、HPLC 分離を実行する前に原液を 100 倍希釈します。</li>
		<li>HPLC クロマト グラム上の各商品には、ピーク面積比 (%) を決定します。</li>
		<li>次の式に従って各化合物のモル吸収率の比率を計算します。 Ε2 : ε3 : ε4 =2/n2 :3/n3 :4/n4 εはモルの吸収率、A ピーク面積、n モルの重量。</li>
	</ol>
</li>
	<li>次の数式によると担体を計算します。 n2 : n3 : n4 =2/ε2 :3/ε3 :4/ε4
</li>
</ol>

著者は何も明らかに異常であります。

1-Iodoalkynes、1, 2-diiodoalkenes と 1,1,2 triiodoalkenes は、chemoselectively 酸化 iodination(s) 効率的な仲介人として超原子価ヨウ素試薬を用いる合成をすることができます。これらの化学選択的ヨウ素プロトコルの最も重要な要因は、自然と溶媒と同様、ヨウ素ソースの読み込みです。たとえば、1 iodoalkyne 2は、主要な製品 (52% の利回り) として得られたとき TBAI (2.5 当量読み込み) は溶媒として?...

Iodoalkynes と iodoalkenes は、広く使用されている重要な前駆体と有機合成1,2,3,4, 生理活性物質内のビルディング ブロックの合成に有用な材料と複雑な分子 C を変換の容易さを与え-私は5,6,7、8を結合します。近年、末端アルキンの酸化ヨウ素は、iodoalkyne および iodoalkene 誘導体の合成により多くの注目を集めています。金属触媒9,10、11,12, 超原子価ヨードニウム触媒13,14, 陽極酸化システムを使用して、これまでのところ、効率的な方法15、イオン液体系16KI (または2)-酸化剤組み合わせ17,18,19,20, 超音波21, 相間移動触媒22、 N- iodosuccinimide9,22,23,24,25, n- バリ26,27,28,29,30,31、グリニャール試薬32モルホリン触媒17,33,24,35は、アルキンのヨウ素のために開発されています。最近では、1 iodoalkynes、1, 2-diiodoalkenes と 1,1,2-triiodoalkenes の36の合成のための実用的なおよび化学選択的プロトコルを報告しています。このメソッドの機能は、緑と実用的な: (1) 超原子価ヨウ素触媒の酸化機能化試薬としての毒性が低い他従来重い金属系酸化剤37,38と比較して 39,40,41,42, および (2) TBAI KI はヨウ素のソースとして使用されます。さらに、私たちのシステムは温和な条件下で優れた選択性を与えます。1-iodoalkynes、1, 2-diiodoalkenes と 1,1,2-triiodoalkenes の化学選択的合成は、組成物、オキシダント、沃素源溶媒など、さまざまな要因を正確に制御を必要です。これらのうち、ヨウ素ソースは反応の担体の最も重要な要因です。いくつかの種類のスクリーニングおよびヨウ素のソースとして、溶剤の荷重後、3 つの方法は識別され、設立されました。まず、PIDA (TBAI PIDA) との組み合わせでのヨウ素源として TBAI は 1 iodoalkynes の合成のための選択。また、1, 2-diiodoalkenes がキ PIDA システムを使用して効率的に得られます。両方の方法は、高収率と高い担体に対応する製品を買う余裕します。対応するトライ iodinationproducts、すなわち。、1,1,2-triiodoalkenes、TBAI PIDA と KI PIDA システム36を組み合わせるワンポット合成から良好な収率で得られました。
ここでは、デモンストレーションを末端アルキンのヨウ素の担体が 1 iodoalkynes から操縦ことができる 1, 2-diiodoalkenes と 1,1,2-triiodoalkenes と同様の反応条件下でどのようにことができる正確なコントロールを強調表示酸化剤、ヨウ素のソース、および溶媒を慎重に選択するによって出されます。この新しい合成手法の開発、 ptolylethyne モデル基板として使用しています。次のプロトコルの 1-(iodoethynyl)-4 合成に焦点を合わせる-ベンゼン、(E)-1-(1,2-diiodovinyl)-4-ベンゼン、1-メチル - 4-(1,2,2-triiodovinyl) ベンゼン、これらの化合物は 1-iodoalkynes、1, 2-のための代表diiodoalkenes と 1,1,2-triiodoalkenes、それぞれ、すなわちプロトコルは、広い範囲、および芳香族および脂肪族末端アルキン36の化学選択的ヨウ素に同じ手法を適用できます。
試薬は末端アルキンの化学選択的ヨウ素の採用し、技術からの小さい偏差は対象製品に関して劇的な違いに結果を記載しました。例えば、KI および溶媒の CH3CN から CH3CN H2O に変更する TBAI からヨウ素ソースの変更ヨウ素の担体に劇的な影響を持っています。詳しいプロトコルは 1-iodoalkynes、1, 2-diiodoalkenes と 1,1,2-triiodoalkenes の合成の際に多くの一般的な落とし穴を避けるために末端アルキンの化学選択的ヨウ素とこの分野での新しい実践を支援することを目指しています。

<table border="0" cellpadding="0" cellspacing="0" width="860">
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			<td></td>
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</table>

chemoselective preparation of 1-iodoalkynes, 1,2-diiodoalkenes, and 1,1,2-triiodoalkenes based on the oxidative iodination of terminal alkynes

提案する化学選択的合成 1-(iodoethynyl)-4-1-(1,2-diiodovinyl)-4-ベンゼン、ベンゼン、1-メチル - 4-(1,2,2-triiodovinyl) 1 iodoalkynes の実用的な化学選択的準備のための代表的な例としてベンゼン、1, 2-diiodoalkenes と 1,1,2-triiodoalkenes 超原子価ヨウ素試薬による末端アルキンの化学選択的ヨウ素から。担体は、画面のヨウ素源および/または超原子価ヨウ素試薬の様々 なモデルの基板としてptolylethyne を使用して確認されました。氣、PIDA の組み合わせは、1, 2-diiodoalkenes を生成し、ヨウ化テトラブチル アンモニウム (tbai を用いた), (diacetoxyiodo) ベンゼン (PIDA) の組み合わせは選択的に 1-iodoalkynes を生成します。TBAI PIDA と KI PIDA の両方に基づいてワンポット合成には、対応する 1,1,2-triiodoalkenes が得られます。これらのプロトコルは、総合的重要な芳香族と脂肪族の 1 iodoalkynes、1, 2-diiodoalkenes および 1,1,2-triiodoalkenes は、優れた担体と良好な収率で得られた合成に適用された後。

1-iodoalkynes、1, 2-diiodoalkenes と 1,1,2 triiodoalkenes ptolylethyne の酸化ヨウ素化に基づく化学選択的合成は、図 1のとおりです。すべての反応は、空気にさらされました。本研究ではすべての化合物は1H と13C の NMR 分光法、質量分析法、製品の構造および反応の選択性にアクセスし、純度を探索する高速液体クロマトグラフィーにより特徴づ?...

Watch this Scientific Journal Video about Chemoselective Preparation of 1-Iodoalkynes, 1,2-Diiodoalkenes, and 1,1,2-Triiodoalkenes Based on the Oxidative Iodination of Terminal Alkynes at JoVE.com

Chemoselective Preparation of 1-Iodoalkynes, 1,2-Diiodoalkenes, and 1,1,2-Triiodoalkenes Based on the Oxidative Iodination of Terminal Alkynes

1-Iodoalkynes、1, 2-Diiodoalkenes、末端アルキンの酸化ヨウ素化に基づく 1,1,2 Triiodoalkenes の化学選択的準備

ここで、超原子価ヨウ素試薬を用いる末端アルキンの酸化ヨウ素のための詳しいプロトコルが表示された、1 iodoalkynes、1, 2-diiodoalkenes と 1,1,2-triiodoalkenes が chemoselectively を買う余裕します。

We present the chemoselective synthesis of 1-(iodoethynyl)-4-methylbenzene, 1-(1,2-diiodovinyl)-4-methylbenzene, and ...

chemoselective-preparation-1-iodoalkynes-12-diiodoalkenes-112

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Alkynes

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7.6K ビュー.  Guangdong University of Technology. ここで、超原子価ヨウ素試薬を用いる末端アルキンの酸化ヨウ素のための詳しいプロトコルが表示された、1 iodoalkynes、1, 2-diiodoalkenes と 1,1,2-triiodoalkenes が chemoselectively を買う余裕します。

ビデオ: Chemoselective Preparation of 1-Iodoalkynes, 1,2-Diiodoalkenes, and 1,1,2-Triiodoalkenes Based on the Oxidative Iodination of Terminal Alkynes

Methods to Identify the NMR Resonances of the 13C-Dimethyl N-terminal Amine on Reductively Methylated Proteins

Nuclear magnetic resonance (NMR) spectroscopy is a proven technique for protein structure and dynamic studies. To study proteins with NMR, stable magnetic isotopes are typically incorporated metabolically to improve the sensitivity and allow for sequential resonance assignment. Reductive 13C-methylation is an alternative labeling method for proteins that are not amenable to bacterial host over-expression, the most common method of isotope incorporation. Reductive 13C-methylation is a chemical reaction performed under mild conditions that modifies a protein&#39;s primary amino groups (lysine &#949;-amino groups and the N-terminal &#945;-amino group) to 13C-dimethylamino groups. The structure and function of most proteins are not altered by the modification, making it a viable alternative to metabolic labeling. Because reductive 13C-methylation adds sparse, isotopic labels, traditional methods of assigning the NMR signals are not applicable. An alternative assignment method using mass spectrometry (MS) to aid in the assignment of protein 13C-dimethylamine NMR signals has been developed. The method relies on partial and different amounts of 13C-labeling at each primary amino group. One limitation of the method arises when the protein&#39;s N-terminal residue is a lysine because the &#945;- and &#949;-dimethylamino groups of Lys1 cannot be individually measured with MS. To circumvent this limitation, two methods are described to identify the NMR resonance of the 13C-dimethylamines associated with both the N-terminal &#945;-amine and the side chain &#949;-amine. The NMR signals of the N-terminal &#945;-dimethylamine and the side chain &#949;-dimethylamine of hen egg white lysozyme, Lys1, are identified in 1H-13C heteronuclear single-quantum coherence spectra.

Methods to Identify the NMR Resonances of the 13C-Dimethyl N-terminal Amine on Reductively Methylated Proteins

Two methods for assigning the &#945;- and &#949;-dimethylamine nuclear magnetic resonance signals of a reductively 13C-methylated N-terminal lysine are described. One method utilizes the pH-induced selectivity of the reductive methylation reaction, and the other uses aminopeptidase to selectively remove the N-terminal lysine.

Nuclear magnetic resonance (NMR) spectroscopy is a proven technique for protein structure and dynamic studies. To study proteins with NMR, stable magnetic ...

化学

Determining the Ice-binding Planes of Antifreeze Proteins by Fluorescence-based Ice Plane Affinity

Antifreeze proteins (AFPs) are expressed in a variety of cold-hardy organisms to prevent or slow internal ice growth. AFPs bind to specific planes of ice through their ice-binding surfaces. Fluorescence-based ice plane affinity (FIPA) analysis is a modified technique used to determine the ice planes to which the AFPs bind. FIPA is based on the original ice-etching method for determining AFP-bound ice-planes. It produces clearer images in a shortened experimental time. In FIPA analysis, AFPs are fluorescently labeled with a chimeric tag or a covalent dye then slowly incorporated into a macroscopic single ice crystal, which has been preformed into a hemisphere and oriented to determine the a- and c-axes. The AFP-bound ice hemisphere is imaged under UV light to visualize AFP-bound planes using filters to block out nonspecific light. Fluorescent labeling of the AFPs allows real-time monitoring of AFP adsorption into ice. The labels have been found not to influence the planes to which AFPs bind. FIPA analysis also introduces the option to bind more than one differently tagged AFP on the same single ice crystal to help differentiate their binding planes. These applications of FIPA are helping to advance our understanding of how AFPs bind to ice to halt its growth and why many AFP-producing organisms express multiple AFP isoforms.

Antifreeze proteins (AFPs) bind to specific planes of ice to prevent or slow ice growth. Fluorescence-based ice plane affinity (FIPA) analysis is a modification of the original ice-etching method for determination of AFP-bound ice planes. AFPs are fluorescently labeled, incorporated into macroscopic single ice crystals, and visualized under UV light.

蛍光ベースの氷面アフィニティーによる不凍タンパク質の氷結合平面の決定

Antifreeze proteins (AFPs) are expressed in a variety of cold-hardy organisms to prevent or slow internal ice growth. AFPs bind to specific planes of ice ...

Preparation and Use of Carbonyl-decorated Carbenes in the Activation of White Phosphorus

Here we present a protocol for the synthesis of two distinct carbonyl-decorated carbenes. Both carbenes can be prepared using nearly identical procedures in multi-gram scale quantities. The goal of this manuscript is to clearly detail how to handle and prepare these unique carbenes such that a synthetic chemist of any skill level can work with them. The two carbenes described are a diamidocarbene (DAC, carbene 1) and a monoamidoaminocarbene (MAAC 2). These carbenes are highly electron-deficient and as such display reactivity profiles that are atypical of more traditional N-heterocyclic carbenes. Additionally, these two carbenes only differ in their electrophilic character and not their steric parameters, making them ideal for studying how carbene electronics influence reactivity. To demonstrate this phenomenon, we are also describing the activation of white phosphorus (P4) using these carbenes. Depending on the carbene used, two very different phosphorus-containing compounds can be isolated. When the DAC 1 is used, a tris(phosphaalkenyl)phosphane can be isolated as the exclusive product. Remarkably however, when MAAC 2 is added to P4 under identical reaction conditions, an unexpected carbene-supported P8&#160;allotrope of phosphorus is isolated exclusively. Mechanistic studies demonstrate that this carbene-supported P8allotrope forms via a [2+2] cycloaddition dimerization of a transient diphosphene which has been trapped by treatment with 2,3-dimethyl-1,3-butadiene.

Here, we present a protocol for the synthesis of two carbonyl-decorated carbenes. The protocol makes these interesting compounds readily available to chemists of all skill levels. In addition to the synthesis of these two carbenes, their use in the activation of white phosphorus is also described.

白リンの活性化カルボニル装飾カルベンの調製および使用

Here we present a protocol for the synthesis of two distinct carbonyl-decorated carbenes. Both carbenes can be prepared using nearly identical procedures ...

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

リン酸化ペプチドの強化充実のためのマクロポーラスポリマーモノリスの高度に多孔性配位高分子コーティングの製造

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr2+ act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air.

化学溶液法によるシリコン上のマクロポーラスエピタキシャル石英薄膜の作製

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide (CdSe@CdS) nanorod photocatalysts. Seeded rods are grown using a colloidal hot-injection method and then moved to an aqueous medium by ligand exchange. CdSe@CdS nanorods, an iridium precursor and other salts are mixed and illuminated. The deposition process is initiated by absorption of photons by the semiconductor particle, which results with formation of charge carriers that are used to promote redox reactions. To insure photochemical oxidative growth we used an electron scavenger. The photogenerated holes oxidize the iridium precursor, apparently in a mediated oxidative pathway. This results in the growth of high quality crystalline iridium oxide particles, ranging from 0.5 nm to about 3 nm, along the surface of the rod. Iridium oxide grown on CdSe@CdS heterostructures was studied by a variety of characterization methods, in order to evaluate its characteristics and quality. We explored means for control over particle size, crystallinity, deposition location on the CdS rod, and composition. Illumination time and excitation wavelength were found to be key parameters for such control. The influence of different growth conditions and the characterization of these heterostructures are described alongside a detailed description of their synthesis. Of significance is the fact that the addition of iridium oxide afforded the rods astounding photochemical stability under prolonged illumination in pure water (alleviating the requirement for hole scavengers).

A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

CdSeの@のCdSナノロッド上にイリジウム酸化物ナノ粒子の光化学酸化成長

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

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.

調製と<em&gt;インビトロ</em&gt;磁気共鳴イメージングのためのデンドリマーベースの造影剤のキャラクタリゼーション

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

Preparation of Chitosan-based Injectable Hydrogels and Its Application in 3D Cell Culture

The protocol presents a facile, efficient, and versatile method to prepare chitosan-based hydrogels using dynamic imine chemistry. The hydrogel is prepared by mixing solutions of glycol chitosan with a synthesized benzaldehyde terminated polymer gelator, and hydrogels are efficiently obtained in several minutes at room temperature. By varying ratios between glycol chitosan, polymer gelator, and water contents, versatile hydrogels with different gelation times and stiffness are obtained. When damaged, the hydrogel can recover its appearances and modulus, due to the reversibility of the dynamic imine bonds as crosslinkages. This self-healable property enables the hydrogel to be injectable since it can be self-healed from squeezed pieces to an integral bulk hydrogel after the injection process. The hydrogel is also multi-responsive to many bio-active stimuli due to different equilibration statuses of the dynamic imine bonds. This hydrogel was confirmed as bio-compatible, and L929 mouse fibroblast cells were embedded following standard procedures and the cell proliferation was easily assessed by a 3D cell cultivation process. The hydrogel can offer an adjustable platform for different research where a physiological mimic of a 3D environment for cells is profited. Along with its multi-responsive, self-healable, and injectable properties, the hydrogels can potentially be applied as multiple carriers for drugs and cells in future bio-medical applications.

Here we describe a facile preparation of chitosan-based injectable hydrogels using dynamic imine chemistry. Methods to adjust the hydrogel&#8217;s mechanical strength and its application in 3D cell culture are presented.

キトサンを用いた注射ゲルおよび 3 D 細胞培養への応用の準備

The protocol presents a facile, efficient, and versatile method to prepare chitosan-based hydrogels using dynamic imine chemistry. The hydrogel is ...

Scale-up Chemical Synthesis of Thermally-activated Delayed Fluorescence Emitters Based on the Dibenzothiophene-S,S-Dioxide Core

We report a procedure to linearly scale-up the synthesis of 2,8-bis(3,6-di-tert-butyl-9H-carbazol-9-yl)dibenzothiophene-S,S-dioxide (compound 4) and 2,8-bis(10H-phenothiazin-10-yl)dibenzothiophene-S,S-dioxide (compound 5) using Buchwald-Hartwig cross-coupling reaction conditions. In addition, we demonstrate a scaled-up synthesis of all non-commercially available starting materials that are required for the amination cross-coupling reaction. In the present article, we provide the detailed synthetic procedures for all of the described compounds, alongside their spectral characterization. This work shows the possibility to produce organic molecules for optoelectronic applications on a large scale, which facilitates their implementation into real world devices.

Scale-up synthesis of highly efficient thermally activated delayed fluorescence emitters is described in the presented article.

スケール アップ ジベンゾチオフェン S、S 二酸化コアに基づく熱重合遅延蛍光体の化学合成

We report a procedure to linearly scale-up the synthesis of 2,8-bis(3,6-di-tert-butyl-9H-carbazol-9-yl)dibenzothiophene-S,S-dioxide (compound 4) and ...

Preparation of Polyoxometalate-based Photo-responsive Membranes for the Photo-activation of Manganese Oxide Catalysts

This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic polymers, with the aim of photo-activating oxygen-evolving manganese oxide catalysts, which are important components in artificial photosynthesis. The cross-linking technique was applied to obtain a self-standing membrane with a high PW12O403- content. Incorporation and structure retention of PW12O403- within the polymer matrix were confirmed by FT-IR and micro-Raman spectroscopy, and optical characteristics were investigated by UV-Vis spectroscopy, which revealed successful construction of the metal-to-metal charge transfer (MMCT) unit. After deposition of MnOx oxygen evolving catalysts, photocurrent measurements under visible light irradiation verified the sequential charge transfer, Mn &#8594; MMCT unit &#8594; electrode, and&#160;the photocurrent intensity was consistent with the redox potential of the donor metal (Ce or Co). This method provides a new strategy for preparing integrated systems involving catalysts and photon-absorption parts for use with photo-functional materials.

Here, we present a protocol to prepare charge transfer chromophores based on a polyoxometalate/polymer composite membrane.

マンガン酸化物触媒の光活性化用ポリ酸を用いた光応答性膜の作製

This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic ...