現在の仕事は、Vicerrectoría ・ デ ・危惧 y プロジェクト号、科学の漏洩 BUAP から領土・ デ ・ Posgrado によってサポートされています。REOY-NAT14、15、16-G. 砥-NAT17。RMG は CONACyT (メキシコ) の奨学金 417887 をありがちましょう。

1. 反応
<ol><li>発煙のフード 0.5 mol (29.8 mL) 氷酢酸と開かれたラウンド 100 mL フラスコを配置し、3, 5-dimethylpyridine と H2O2 (35%) 5 mL 0.051 mol (5.82 mL) を追加します。5 h で 80 ° C の内部温度で一定の電磁攪拌下で混合物の反応をしてください。</li>
	<li>反応時間後氷 (氷酢酸ガスを公開を行う)、24 ° C に、フラスコを冷却し、過剰の酢酸を削除する 90-120 分間高真空蒸留ユニットに差し込みます。 注意: は、ホット マテリアルを使用しないでください。ガラス管理可能な温度に達するまで待機します。また、これは常圧蒸留装置の上部に入る蒸気を避けます。</li>
	<li>できるだけ多く酢酸の混合物に集中して痕跡の除去を確実に 2 回蒸留水 (10 mL) を追加します。</li>
</ol>2. 塩基度調整と抽出
<ol><li>Bi 芳醇水に分離の粘性と透明の製品を溶解し、純粋な固体 Na2CO310 pH 調整にポテンショメータを使用します。</li>
	<li>250 mL 分離漏斗で慎重にソリューションを配置し、5 回収穫を改良する CHCl3 250 mL で抽出します。有機層を回復し、固体の Na2以上だから乾燥 30 分、最大の製品が含まれる4 。必要に応じて、再 CHCl3の希望の金額で水相を抽出します。 注意: CHCl3は眠気やめまい; を引き起こす可能性があります。ケアとヒューム フードの中を処理します。</li>
	<li>非常に吸湿性のクリア ベージュ結晶性粉末 (70%) を形成するまで高真空蒸留装置で減圧下で溶媒を削除します。</li>
</ol>3. 結晶化過程
<ol><li>冷たい高実行される液体クロマトグラフィー (HPLC) グレード ジエチル エーテル 50 mL で結晶性の粉末の 4.3 g を溶解します。真空フィルター固体原料または塵のすべてのトレースを削除するソリューションです。濾液をガラス シャーレに注ぎ、研究所の冷蔵庫に 4 ° C で蒸発を遅らせるためにそれを残してします。</li>
	<li>2 日後、明確な無色の結晶が得られることを確認します。310 311 K の範囲にあるべき融点を測定し</li>
</ol>4. 3, 5-ルチジンn-酸化物 Dehydrate の解析
<ol><li>さらに x 線分析用フラスコの壁からデカンテーションによってして角柱形状および無色に形成される結晶を削除します。直後ではなくを使用する場合は、結晶にジエチル エーテル結晶水和を避けるためにしてください。</li>
	<li>0.010 g 3, 5-ルチジンN酸化物の NMR H1と C13分析手順の有効性を証明するために行うため CDCl3 0.4 mL に脱水を解消します。</li>
</ol>

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ここで提示されたプロトコルは、基板上の官能基化法として 3, 5-ルチジンの窒素原子に酸素原子をリンクする従来方法です。この手法は、x 線の適切な脱水の結晶 (図 5、DSC HX300 サイバー ショット ソニーのカメラで撮影した画像) を生成する確立も。限り我々 が懸念している、ない多くのレポートは、このような結晶16の生産を説明しています。多くの化合物は、彼らは様々 な金属17,18,19,20キレートは、ときに x 線分析用理想的な結晶を成長させます。作成された結晶状の粉末は、北里フラスコとブフナーを使用して彼らの母液から抽出することが重要です。ホースを使用して、北里フラスコ、真空ラインに接続されている、それの上に、ブフナーは、濾紙で配置されます。真空をオンには、フィルター ペーパーは製品の結晶化の溶媒の少量で湿らせた。これは、結晶性の粉末が真空の効果によって、ブフナーにしたたるを防ぎます。ろ紙を確保した後に結晶状の粉末がフィルター処理し、フラスコの底に、どれも確実に結晶状の粉末を含むソリューションが揺れています。ソリューションは、ブフナー上すぐに注がれています。フィルター紙の上約 10 分間得られる結晶性の粉末が残っていると真空がオフになっているし、結晶状の粉末は紙から超然し不透明なガラス瓶で保存されている、そのコードの付いた、さらなる分析まで 4 ° C で保管します。濾液は、ガラス シャーレ、x 線分析のための十分な結晶の形成を改善するために 4 ° C で蒸発徐々 にそれを残しに注がれています。
溶剤や材料入手が容易、一般に任意の研究所で発見されるこのプロトコルを使用することに注意してくださいすることが重要です。Na2CO3と一貫性のある磁気攪拌の添加により pH 調整は最終製品の収量に重要です。ただし、すべてのプロセス ステップで、出発原料のトレースする必要がありますないが存在する結晶性の粉末とその後結晶の形成を余裕の抽出段階で特に特別な注意を払うことが重要です。このように、製品の品質を確保するため NMR や IR 分光法によるこの抽出/精製段階を監視できます。
このプロトコルの再現性を確保するため NMR は優れたツールです。細かい詳細はスペクトルに表示されます。すべての信号は、図 1のくぼみとして表示されます。これらのくぼみは分割、すべての信号のすなわち多様性を明確に描かれています。陽子 b のインスタンス (Jディップb 〜 0.75 Hz) 信号は、それらの間の分離の頂上で 4 つのピーク (Δピーク) ムカムカ定数を表示 〜 0.0075 ppm。0.0075 ppm 次方程式21を使用してエネルギーに変換するもの
<img alt="Equation 1" src="/files/ftp_upload/57233/57233eq1.jpg">式 1
<img alt="Equation 2" src="/files/ftp_upload/57233/57233eq2.jpg">
変換は展開信号は、メチル基の 3 つの水素原子核の中で双極子の空間的相互作用から来るので、にもかかわらず、彼らは、c とは、彼らのプロトンと 4 つの単一結束よりもさらにお勧めを感知することができますその双極子磁気モーメント相互作用22とします。また、プラスフリーシグマ メチル グループの回転を結合できます信号の多様性で表示する超超微細陽子相互作用です。陽子の septuplets、6.9 7.9 ppm で c はそれぞれ同じ双極子自然現象から派生されます。これらの場合、陽子、c は同じ回転動的のメチル基のプロトンを区別できると。最後に、期待どおり、計算されるJディップに a、b、c は、ほとんど同じ値を持っていると 〜 0.75 Hz。相互作用のこれらの量は水素核磁気異方性の中で空間的な整理を確認します。
その一方で、 1 C2 vの対称性と同等の炭素23になります。図 2、 13C スペクトルは、18 ppm の炭素 d 芳香環に接続されているメチル グループの典型的な信号を示しています。また、129 ppm 信号はより少なく陰性の要素の影響を炭素のためこの地域を表示します。高周波磁場により多くの露出の炭素核の信号は 137 ppm22に掲載されています。
説明されている方法は合成ピリジン n-オキシド、ソフトの反応条件と安価で簡単なアクセスの試薬、その他の触媒を必要としない合理的な時間で、良好な収率を提供のため非常に便利です。これらの条件は、科学的な教育コミュニティのため興味の他の分子の前駆体としてピリジン n-オキシドの広範な範囲を取得する使用できます。適切な方法論では、学生の成功の合成化合物と結晶の形成を確認する幸福を証明するため教育研究所の基本的な実験および概念的なツールを取得する機会を与えます。ただし、任意の化学反応のような一般的に使用する試薬は危険なので、すべての予防措置を取る必要があることを強調することが重要です。

今日では、世界中の科学者に投資しているリソース低反応性フロント付加反応1,2に知られている、芳香族グループの機能化の新しい合成ルートの開発 3。窒素原子は炭素原子を置換、ピリジンはリング3炭素原子のみで構成されるアナログに似たような反応を示し、それは通常追加ではなく、置換の機構を受けます。N-酸化物、窒素および酸素原子3空軌道を持つ窒素の非共有結合電子対の重複によって形成される酸素ドナーの絆の存在によって特徴的な。特に、ピリジンN-酸化物は、ルイス塩基、電子供与体として作用する可能性、N-O 部位と彼らは対応するルイス酸・塩基対を形成するルイス酸と組み合わせることがあります。潜在的な求電子剤に向かってルイス酸の nucleophilicity を増加できることが条件の下で反応させる、通常の反応は発生しませんので、不可欠な化学結果しております。おそらくこのような化合物の最も頻繁に使用は様々 な酸化反応酸化剤4として動作です。ピリジンN-酸化物とそのリング官能基化誘導体の多くは生物学的活性や薬理学的エージェント5、再発の分子であり、さまざまな分光学的ツールによる明確な空間分布を確立されています。それらのいくつかの6,7。ピリジン環に異なるグループを関連付けて研究の科学者はイソキサゾリン フォーム 6 - キシレンを沸騰 DBU などベースの触媒量を必要とするので、簡単で従来の方法を生成するさまざまな方法論をテストしています。置換-2-アミノピリジンN-酸化物8,9。種々 のピリジン誘導体は彼らの対応するNに変えられた-マンガン量を触媒の存在下で酸化物 tetrakis(2,6-diclorophenyl) CH2Cl2/CH3ポルフィリンおよびアンモニウムのアセテートCN8,10。CH2Cl2 methyltrioxorhenium8、11、または過剰なジメチルジオキシランの添加による触媒量の存在下で H2O2を使用して酸化物に酸化する他のピリジン0 の ° C で対応するNにつながる-酸化物8,12,13,14。ビス (トリメチルシリル) 過酸化 CH2Cl2で trioxorhenium の存在下ではピリジンNの合成使用されています-酸化物8,11。アミノピリジンNの合成-カロの酸 (peroxomonosulfuric 酸) を使用して含むアシル化もされて酸化物報告8。それにもかかわらず、ここでは、報告された方法論と落合1、によって報告された方法論の一部を使用してアクセスできる安価な試薬、H2O2氷酢酸の使用で非常に良い結果を提供します。この実習は第三級アミンに作用する大規模な準備での使用に適して、それのみ 30% 過酸化水素が必要な反応で良好な収率と 70 から 80 ° C 間の温度で氷酢酸を生成および浄化プロセスが使用触媒や高価な試薬1を使用せず、蒸留のようなほとんどの合成実験室で利用可能です。文献は、他の方法論も多く、10-24 h と温度が 100 ° C 4,8からのタイム フレームと結晶 x 線解析では収量はほとんど報告を報告します。
受身に様々 なn-酸化誘導体、適切に求核または求電子のいずれかの方法でルチジン リングをアクティブに使用されます。求または求電子的要因は、置換基の影響を受けます。主な要因は、電子グループ ピリジン環、求核特性1となっています。無料のN-酸化化合物は芳香環の非局在電荷による x 線解析に適した結晶としてほとんど分離されます。しかし、溶媒和要因は酸素15の負の密度を安定させるために重要です。

<table border="0" cellpadding="0" cellspacing="0" style="width:725px;" width="725">
	<colgroup>
		<col />
		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:212px;">3,5-lutidine</td>
			<td style="width:228px;">Sigma-Aldrich</td>
			<td style="width:119px;">L4206-500ML</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Glacial acetic acid</td>
			<td>Fermont</td>
			<td>3015</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Hidrogen peroxide (35%)</td>
			<td>Sigma-Aldrich</td>
			<td>349887-500ML</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Na2CO3 anhydrous</td>
			<td>Productos Qu&#237;micos Monterrey</td>
			<td>1792</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Na2SO4 anhydrous</td>
			<td>Alfa reactivos</td>
			<td>25051-C</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">CHCl3</td>
			<td>Fermont</td>
			<td>6205</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Ethyl eter</td>
			<td>Mercury Chemist</td>
			<td>QME0309</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Distilled water</td>
			<td>Comercializadora Qu&#237;mica Poblana</td>
			<td>not-existent</td>
			<td></td>
		</tr>
	</tbody>
</table>

syntheses, crystallization, and spectroscopic characterization of 3,5-lutidine n-oxide dehydrate

3, 5-ルチジンN酸化物の合成は、脱水、 12-アミノ-ピリジン-3, 5-ジカルボン酸の合成ルートで達成されました。落合最初 12 h プロセスで 1957 年に非置換ピリジンの方法論に使用がない適切な結晶を x 線が得られました。ここで紹介する方法で使用される代替のリングは、 1で異なる求強度を付与する非対称単位に水分子の付加を明確に影響。X 線結晶化合物1は 2 つの水分子の存在によって酸素の負電荷の安定化により水素原子がリングに正電荷を寄付このような水の分子も超分子的相互作用を構築するサービスを提供します。水和物の分子は、10 の pH を調整することによって到達できるアルカリ用も可能です。二重メチル置換リングと 5 h の反応時間で重要なより汎用性の高い方法になりますと将来リング挿入用の広い化学。

プロトコルは、本質的に落合の技術1の拡張です。ただし、温度が低いとより少ない時間が適用されます。この単純なメソッドを使用して、置換ピリジンNである汎用性の高いリガンドを取得できます-酸化物の派生物。1の形成を確認するには、手順の有効性をテストする NMR 1H と13C 分析を優先します。
化学シフトは、 1の形成を示しています。2.28 ppm 信号 (につき部分百万) 永久磁気よりも少ない割合で磁場を感知 3 と 5 の位置で 2 つのメチル グループの六つの等価水素に対応します。Septuplets の 2 つのセットがある: 1 つは 7.9、2 倍になる図 1位置 a のプロトンに属する 6.9 で他の信号のサイズを示します化学シフト酸素原子 bonde の存在によって誘発されるで c 位置のプロトンに属するピリジン環の窒素原子に d。酸素原子は電気撤退と酸素原子に近い水素原子 (メチル水素 (b) よりも高い周波数に c と) ショーの変位。
同じプロセスは図 2、NMR 13C スペクトルについてプロットされますどこ酸素原子に近い炭素の信号 (c と) Δcの信号間の周波数分離を表示 = 1,300 Hz と Δ、 200 Hz を =。もう一度、メチル炭素では、変更は表示されません。IR スペクトルを使用して、メソッドと同様の成功を参照してくださいできます。
得られた ORTEP 図、図 4は、非対称分子を取り巻く水の 2 つの分子の存在を示しています。これらの分子は、N-O 結合を安定化すると考えられています。同様のケースではピリジンNの記載されている-酸化物および関連芳香族酸化物。そこは重要な 1 と孤立電子対の電子の数よりも高く計算される結合次数の 3 よりも低い酸素原子に反映 π 型 O→N バック-寄付を安定化6。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/57233/57233fig1.jpg"> 図 1.TMS CDCl3 500 MHz NMR 1H 1 のスペクトルを参照します。統合と 3 つのシグナルの化学シフト lutine Nで現在の水素原子の 3 つの種類に同意する-酸化物。<a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57233/57233fig1large.jpg" target="_blank">この図の拡大版を表示するのにはここをクリックしてください</a>。
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/57233/57233fig2.jpg"> 図 2.TMS CDCl3 100 MHz NMR 13C 1 のスペクトルを参照します。3 つの信号は 5 つの芳香族炭素と 2 つのメチル グループの 1 つのために観察されます。<a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57233/57233fig2large.jpg" target="_blank">この図の拡大版を表示するのにはここをクリックしてください</a>。
<img alt="Figure 3" class="xfigimg" src="/files/ftp_upload/57233/57233fig3.jpg"> 図 3.1 の IR スペクトル。O H 債、上記 3,300 cm-1、超分子の構造形成と結晶の形成を担当しています。<a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57233/57233fig3large.jpg" target="_blank">この図の拡大版を表示するのにはここをクリックしてください</a>。
<img alt="Figure 4" class="xfigimg" src="/files/ftp_upload/57233/57233fig4.jpg"> 図 4.1 H2O フォームの 2 つの分子が水素結合ルチジンの酸素は、酸素原子に水素原子を運転をブリッジの得られた ORTEP 図。この図は、メリノ ・ ガルシアらから変更されています。12<a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57233/57233fig4large.jpg" target="_blank">この図の拡大版を表示するのにはここをクリックしてください</a>。
<img alt="Figure 5" class="xfigimg" src="/files/ftp_upload/57233/57233fig5.jpg"> 図 5.1 ジエチル エーテル (top)、戸外 (下) の適切な x 線回折による結晶の写真。これらの結晶の x 線回折装置で確認され、traduced され、分子及び結晶構造24,25、で特別な計算プログラムによって洗練された x 線の回折波を示した26,,2728。<a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57233/57233fig5large.jpg" target="_blank">この図の拡大版を表示するのにはここをクリックしてください</a>。

Watch this Scientific Journal Video about Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate at JoVE.com

Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

症例、ピリジンNの古典的な合成とは異なるシンプルなプロトコルによって脱水合成と 3, 5-ルチジンN酸化物の結晶性の酸化物。このプロトコルは異なる原料を利用し、新しい溶媒和分子構造、ゆっくりと蒸発させるの下に結晶する反応時間が含まれます。

合成、結晶化、および 3, 5-ルチジンNの分光学的キャラクタリゼーション-酸化物の脱水

The synthesis of 3,5-lutidine N-oxide dehydrate, 1, was achieved in the synthesis route of 2-amino-pyridine-3,5-dicarboxylic acid. Ochiai first used the ...

syntheses-crystallization-spectroscopic-characterization-35-lutidine

Nanyang Technological University

Research

JoVE Journal

Chemistry

Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

8.3K ビュー.  Benemérita Universidad Autónoma de Puebla. 症例、ピリジンNの古典的な合成とは異なるシンプルなプロトコルによって脱水合成と 3, 5-ルチジンN酸化物の結晶性の酸化物。このプロトコルは異なる原料を利用し、新しい溶媒和分子構造、ゆっくりと蒸発させるの下に結晶する反応時間が含まれます。

ビデオ: Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

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.

ペプチド第三級アミドライブラリのスプリット·アンド·プールの合成とキャラクタリゼーション

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

化学

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.

官能化有機金属構造体の合成とキャラクタリゼーション

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

Diffuse Reflectance Infrared Spectroscopic Identification of Dispersant/Particle Bonding Mechanisms in Functional Inks

In additive manufacturing, or 3D printing, material is deposited drop by drop, to create micron to macroscale layers. A typical inkjet ink is a colloidal dispersion containing approximately ten components including solvent, the nano to micron scale particles which will comprise the printed layer, polymeric dispersants to stabilize the particles, and polymers to tune layer strength, surface tension and viscosity. To rationally and efficiently formulate such an ink, it is crucial to know how the components interact. Specifically, which polymers bond to the particle surfaces and how are they attached? Answering this question requires an experimental procedure that discriminates between polymer adsorbed on the particles and free polymer. Further, the method must provide details about how the functional groups of the polymer interact with the particle. In this protocol, we show how to employ centrifugation to separate particles with adsorbed polymer from the rest of the ink, prepare the separated samples for spectroscopic measurement, and use Diffuse Reflectance Fourier Transform Infrared Spectroscopy (DRIFTS) for accurate determination of dispersant/particle bonding mechanisms. A significant advantage of this methodology is that it provides high level mechanistic detail using only simple, commonly available laboratory equipment. This makes crucial data available to almost any formulation laboratory. The method is most useful for inks composed of metal, ceramic, and metal oxide particles in the range of 100 nm or greater. Because of the density and particle size of these inks, they are readily separable with centrifugation. Further, the spectroscopic signatures of such particles are easy to distinguish from absorbed polymer. The primary limitation of this technique is that the spectroscopy is performed ex-situ on the separated and dried particles as opposed to the particles in dispersion. However, results from attenuated total reflectance spectra of the wet separated particles provide evidence for the validity of the DRIFTS measurement.

Formulation of stable, functional inks is critical to expanding the applications of additive manufacturing. In turn, knowledge of the mechanisms of dispersant/particle bonding is required for effective ink formulation. Diffuse Reflectance Fourier Transform Infrared Spectroscopy (DRIFTS) is presented as a simple, inexpensive way to gain insight into these mechanisms.

機能性インク中の分散剤/粒子​​結合機構の反射赤外分光識別を拡散

In additive manufacturing, or 3D printing, material is deposited drop by drop, to create micron to macroscale layers.  A typical inkjet ink is a colloidal ...

A Filter-based Surface Enhanced Raman Spectroscopic Assay for Rapid Detection of Chemical Contaminants

We demonstrate a method to fabricate highly sensitive surface-enhanced Raman spectroscopic (SERS) substrates using a filter syringe system that can be applied to the detection of various chemical contaminants. Silver nanoparticles (Ag NPs) are synthesized via reduction of silver nitrate by sodium citrate. Then the NPs are aggregated by sodium chloride to form nanoclusters that could be trapped in the pores of the filter membrane. A syringe is connected to the filter holder, with a filter membrane inside. By loading the nanoclusters into the syringe and passing through the membrane, the liquid goes through the membrane but not the nanoclusters, forming a SERS-active membrane. When testing the analyte, the liquid sample is loaded into the syringe and flowed through the Ag NPs coated membrane. The analyte binds and concentrates on the Ag NPs coated membrane. Then the membrane is detached from the filter holder, air dried and measured by a Raman instrument. Here we present the study of the volume effect of Ag NPs and sample on the detection sensitivity as well as the detection of 10 ppb ferbam and 1 ppm ampicillin using the developed assay.

A procedure for fabrication and performing the filter-based surface enhanced Raman spectroscopic (SERS) assay for the detection of chemical contaminants (i.e., pesticide ferbam and antibiotic ampicillin) is presented.

化学汚染物質の迅速検出のためのラマン分光アッセイ強化フィルターベースの表面

We demonstrate a method to fabricate highly sensitive surface-enhanced Raman spectroscopic (SERS) substrates using a filter syringe system that can be ...

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.

超分子コロイドの合成とキャラクタリゼーション

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

Site Directed Spin Labeling and EPR Spectroscopic Studies of Pentameric Ligand-Gated Ion Channels

Ion channel gating is a stimulus-driven orchestration of protein motions that leads to transitions between closed, open, and desensitized states. Fundamental to these transitions is the intrinsic flexibility of the protein, which is critically modulated by membrane lipid-composition. To better understand the structural basis of channel function, it is necessary to study protein dynamics in a physiological membrane environment. Electron Paramagnetic Resonance (EPR) spectroscopy is an important tool to characterize conformational transitions between functional states. In comparison to NMR and X-ray crystallography, the information obtained from EPR is intrinsically of lower resolution. However, unlike in other techniques, in EPR there is no upper-limit to the molecular weight of the protein, the sample requirements are significantly lower, and more importantly the protein is not constrained by the crystal lattice forces. Therefore, EPR is uniquely suited for studying large protein complexes and proteins in reconstituted systems. In this article, we will discuss general protocols for site-directed spin labeling and membrane reconstitution using a prokaryotic proton-gated pentameric Ligand-Gated Ion Channel (pLGIC) from Gloeobacter violaceus (GLIC) as an example. A combination of steady-state Continuous Wave (CW) and Pulsed (Double Electron Electron Resonance-DEER) EPR approaches will be described that will enable a complete quantitative characterization of channel dynamics.

This article describes methods for site-directed spin labeling and reconstitution of pentameric ligand-gated channels for Electron Paramagnetic Resonance studies. This protocol can be adapted for any membrane protein. The reconstitution method described here can also be used for patch-clamp measurements of macroscopic and single-channel currents in a defined lipid system.

サイト監督スピン標識および五量体リガンド依存性イオンチャネルのEPR分光研究

Ion channel gating is a stimulus-driven orchestration of protein motions that leads to transitions between closed, open, and desensitized states. ...

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We present methods for depositing and passively manipulating C60 molecules on rippled graphene that advance the pursuit of realizing applications involving 1D C60/graphene hybrid structures. The techniques applied in this exposition are geared towards high vacuum systems with preparation areas capable of supporting molecular deposition as well as thermal annealing of the samples. We focus on C60 deposition at low pressure using a homemade Knudsen cell connected to a scanning tunneling microscopy (STM) system. The number of molecules deposited is regulated by controlling the temperature of the Knudsen cell and the deposition time. One-dimensional (1D) C60 chain structures with widths of two to three molecules can be prepared via tuning of the experimental conditions. The surface mobility of the C60 molecules increases with annealing temperature allowing them to move within the periodic potential of the rippled graphene. Using this mechanism, it is possible to control the transition of 1D C60 chain structures to a hexagonal close packed quasi-1D stripe structure.

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Here we present a protocol for the fabrication of C60/graphene hybrid nanostructures by physical thermal evaporation. Particularly, the proper manipulation of deposition and annealing conditions allow the control over the creation of 1D and quasi 1D C60 structures on rippled graphene.

C60/Graphene ハイブリッド ナノ構造の作製と評価

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We ...

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.

半導体 Gyroidal 金属硫黄フレームワークの結晶化に対するチオール ビルディング ブロックの合成

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

Electrophoretic Crystallization of Ultrathin High-performance Metal-organic Framework Membranes

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and non-porous supports (polymer, ceramic, metal, carbon, and graphene). We developed a novel crystallization technique, which is termed the ENACT approach: the electrophoretic nuclei assembly for the crystallization of highly intergrown thin films (ENACT). This approach allows for a high density of heterogeneous nucleation of MOFs on a chosen substrate via the electrophoretic deposition (EPD) directly from the precursor sol. The growth of well-packed MOF nuclei leads to a highly intergrown polycrystalline MOF film. We show that this simple approach can be used for the synthesis of thin, intergrown zeolite imidazole framework (ZIF)-7 and ZIF-8 films. The resulting 500 nm-thick ZIF-8 membranes show a considerably high H2 permeance (8.3 x 10-6 mol m-2 s-1 Pa-1) and ideal gas selectivities (7.3 for H2/CO2, 15.5 for H2/N2, 16.2 for H2/CH4, and 2655 for H2/C3H8). An attractive performance for C3H6/C3H8 separation is also achieved (a C3H6 permeance of 9.9 x 10-8 mol m-2 s-1 Pa-1 and a C3H6/C3H8 ideal selectivity of 31.6 at 25 &#176;C). Overall, the ENACT process, owing to its simplicity, can be extended to synthesize intergrown thin films of a wide range of nanoporous crystalline materials.

A simple, reproducible, and versatile approach for the synthesis of intergrown, polycrystalline metal-organic framework membranes on a wide range of unmodified porous and non-porous supports is presented.

極薄高性能金属有機性フレームワーク膜の電気泳動の結晶化

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of their interactions with cell membranes, lipid bilayers, and viruses. The hydrophilic ligands make these particles colloidally stable in aqueous solutions and the combination with hydrophobic ligands creates an amphiphilic particle that can be loaded with hydrophobic drugs, fuse with the lipid membranes, and resist nonspecific protein adsorption. Many of these properties depend on nanoparticle size and the composition of the ligand shell. It is, therefore, crucial to have a reproducible synthetic method and reliable characterization techniques that allow the determination of nanoparticle properties and the ligand shell composition. Here, a one-phase chemical reduction, followed by a thorough purification to synthesize these nanoparticles with diameters below 5 nm, is presented. The ratio between the two ligands on the surface of the nanoparticle can be tuned through their stoichiometric ratio used during synthesis. We demonstrate how various routine techniques, such as transmission electron microscopy (TEM), nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA), and ultraviolet-visible (UV-Vis) spectrometry, are combined to comprehensively characterize the physicochemical parameters of the nanoparticles.

Amphiphilic gold nanoparticles can be used in many biological applications. A protocol to synthesize gold nanoparticles coated by a binary mixture of ligands and a detailed characterization of these particles is presented.

親和性金ナノ粒子の合成と特性化

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...