Financial support provided by National Science Foundation (CAREER award CHE-0847262. We thank Vapourtec Ltd and Enwave Optronics for equipment support, and Daniel Daleb of the University of Connecticut for his assistance in construction of the flow cell apparatus.

1.反応モニタリングのための適切な信号を探します<ol><li>すべての出発物質および製品のラマンスペクトルを取得します。 </li><li>オーバーレイスペクトルおよび製品に固有のものである強いバンドを識別します。 </li><li>反応の進行を監視するには、このラマンバンドを使用してください。 1608センチメートルのバンドは-1この場合に選択されました。 </li></ol> 2.フローセルを設定します<ol><li>適切なフローセルを取得します。 6.5ミリメートルの幅、20mmの高さ、および5ミリメートル（ 図2A）のパスの長さ：ここでは以下の寸法のものを使用します。 </li><li>周囲光のない環境を提供して容器にフローセルを置きます。 </li><li>フローセル（この場合は1ミリメートルID PFAチューブ）の入口と出口にチューブを接続します。 </li></ol> 3.フローセルとラマン分光をインターフェース<ol><li> （c）に配置することができる柔軟な光学アセンブリとの適切なラマン分光計を得ますフローセルへの近接性を失います。 </li><li>フローセルアセンブリ（ 図2B）を含むボックスに適切な大きさの開口部を通って光学アセンブリを配置します。 </li><li>それはフローセルに触れるまで光学アセンブリをスライドさせ、その後、〜2mmの隙間を残して、それを引き戻します。 </li><li> 100％アセトンでフローセルを満たします。 </li><li>ラマン分光計をオンにして、連続スキャンモードでスペクトルを取得します。 </li><li>静かに時の光パイプに一部を移動させることにより、レーザーの焦点を合わせます。信号がその最大強度であり、ピークがシャープであり、明確に定義されるまで、ライトパイプを移動してください。 </li></ol><img alt="図2" src="/files/ftp_upload/52393/52393fig2.jpg" /> 図2（a）細胞および使用される（B）ラマンインターフェースをフロー。 <a href="https://www.jove.com/files/ftp_upload/52393/52393fig2large.jpg" target="_blank">大きなVEを見るにはこちらをクリックしてください</a>この図のrsion。 4.試薬および溶剤溶液を製造<ol><li> 50mlのメスフラスコにサリチルアルデヒド（6.106グラム、50ミリモル、1当量）およびアセト酢酸エチル（6.507グラム、50ミリモル、1当量）を追加します。 </li><li> 50ミリリットルの全容量に酢酸エチルを追加し、完全に内容物を混合。 </li><li>磁気撹拌棒を含む20mlのガラスバイアルに貯蔵溶液10mlのアリコートを移します。このバイアル「試薬」をラベル</li><li>酢酸エチル100mlボトル90 mlの場所で。 「溶媒​​」は、このボトルにラベルを付けます。アセトン100mlボトル90 mlの場所で。このボトル「溶媒インターセプトを「ラベル。 </li></ol> 5.フロー装置を準備します<ol><li> 「P1」と「P2」のフローユニットは、少なくとも2つのポンプを持っていることを確認し、それらをラベル付けします。各ポンプの溶媒と試薬入口ラインを識別します。 2つのIに「集める」からの出口ラインと「廃棄物」の行を置きますndividual 100ミリリットルのボトルは、それぞれ、「製品」と「廃棄物」と表示されました。 </li><li>反応器として、加熱されることが可能な10ミリリットル容量PFAコイルを使用しています。 </li><li> PFA反応器コイルの入口に、P1を出たチューブを接続します。 </li><li>リアクトルコイル後3ポートポリエーテルエーテルケトン（PEEK）ティーミキサーをインストールします。 </li><li>リアクトルコイル出口チューブから180°、ティーミキサーにチュ​​ーブから出P2を接続します。ティーミキサーの第3のポートにチューブの部分を接続します。このチューブのもう一方の端には背圧調整器を配置します。 </li><li>フローセルの入力に背圧レギュレータの出力からのラインを接続します。 「廃棄物収集/ &quot;スイッチにフローセルの出力からラインを接続します。 </li><li>プライムP1とP2の両方のための溶媒ラインだけでなく、溶剤と、P1用試薬ライン。試薬瓶に溶媒ボトルからP1用試薬ラインを移動します。 </li><li> P1を用いて、反応器に酢酸エチルを渡します/分2ミリリットルでコイルそれが満たされるまで。 2ミリリットル/ 2分間分の流速で、P2を介してアセトンを渡します。 </li><li> 1ml /分のP1とP2の両方のための溶媒の流量を調整します。 7バールの圧力に背圧レギュレータを設定します。所望の温度に原子炉のコイル温度を設定します。 </li><li> 図3の概略図に示すように機器が設定されているダブルチェック。 </li><li>システムは、一定の温度と圧力に達すると、漏れをチェックした後、反応を実行します。 </li></ol><img alt="図3" src="/files/ftp_upload/52393/52393fig3.jpg" /> 反応モニタリング実験のために使用される機器の構成を図3の回路図。 <a href="https://www.jove.com/files/ftp_upload/52393/52393fig3large.jpg" target="_blank">この図の拡大版をご覧になるにはこちらをクリックしてください。</a> 6.反応をモニター<ol><li>ターク酢酸エチル/アセトン溶媒系のEAのバックグラウンドスキャンは、フローセルを通過します。これは、自動的にすべてのその後のスキャンから差し引かれます。 </li><li>スキャンごとに15秒を取るために分光計を構成する（この場合、ラマン分光計は、10秒の積分時間にボックスカー= 3に設定し、1 =平均しました）。 </li><li> 「試薬」と表示されたガラスバイアルに一斉にピペリジン（0.05ミリリットル、0.05ミリモル、0.1当量）を注入します。 </li><li>徹底的から、スイッチP1を混合した後、「試薬」に出口流「溶媒」に設定する」を収集します。」 </li><li>すべての材料が完全に戻って、「試薬」から、スイッチP1「溶媒」をロードされると、別の30分間の反応器コイルを流れる溶剤を続行します。この時間が経過すると、加熱をオフにします。 </li><li>原子炉のコイル温度が50℃以下に冷却したときに電源を入れて、P1とP2をオフポンプ。 </li></ol> 7.データの分析<ol&gt; <li> 1608センチメートル-1対でスプレッドシート、プロットラマン強度にラマン分光計のデータをエクスポートします時間。 </li><li>条件を最適化するために、反復的に流速および反応器温度の数を横切って反応を行います。 </li><li> 1608センチメートル-1対でのラマン強度のオーバーレイプロット時間。 メモ：高いラマン強度が高く、製品の変換と相関します。 </li></ol> 8.最適化された条件を用いて反応を実行します<ol><li>スクリーニング各種条件（様々な流量/反応器温度）を有する、最高の生成物の変換を得るために最適化された条件を用いて反応を実行します。 </li></ol> 9.商品を分離<ol><li>製品フラスコの内容物を取り出し、氷の100 mlの2 M HClを20 mlを含有するビーカーにそれを注ぎます。 </li><li>酢酸エチル（2 ml）を最小限に抑え、製品のフラスコをすすぎ、ビーカーに移します。 </li><li>氷の混合物を攪拌すべての氷が完全に融解するまで。 </li><li>ヒルシュロート、サイドアームフラスコ、ゴムカラーとゴム真空チューブの長さとろ過システムを設定します。 </li><li> 、真空下で得られた沈殿物をろ過冷ジエチルエーテル（10ml）で洗浄し、それが加熱ランプ（2-3時間）またはドライO下/ N真空下で乾燥することができます。 </li><li>溶媒としてのCDCl 3を 用いて、1 H核磁気共鳴（NMR）分光法により生成物の同定を確認してください。 - 7.40（M、2 H）、7.65（DDD、J = 7.53、4.37、2.60 Hzのδ= 2.73（S、3 H）7.31以下のよう500MHzのNMR分光計のために、3-acetylcoumarinの1 H NMRデータは、2 H）8.51（S、1 H）ppmで、13 C NMRデータ：δ= 30.84（CH 3）117.00（CH）118.56（C）124.86（CH）125.27（CH）130.51（CH）134.68（C）147.74 （CH）155.64（C）159.52（C）195.77（C）ppmです。 </li></ol>

<ol>
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The authors have nothing to disclose.

ラマン分光計は、流量装置とインターフェースすることができる容易さは、反応を監視するための貴重なこのインライン技法を行います。反応変数の数は、ユーザーがより速くオフラインの方法を使用した場合よりも最適化された反応条件に到達することができ、迅速な方法でプローブすることができます。本明細書で説明する技術の適用はまた、適切なバンドを見ることができると仮定す?...

連続フロー処理を使用することにより、化学者は、彼らが安全に、効率的に、かつ容易1,2との化学反応の範囲を行うことができることを見つけています。その結果、フロー化学機器は産業環境でだけでなく、学術機関の研究ラボの両方の反応を実行するための不可欠なツールとなってきています。合成化学変換の多種多様な流反応器3,4において行われてきました。選択の場合、バッチでは動作しない反応が連続流条件5下スムーズに進行することが示されています。反応の最適化と品質管理の両方のために、フロー処理のインライン反応モニタリングの取り込みは、重要な利点を提供しています。インライン監視は、実際のサンプル条件にリアルタイム応答で連続分析を提供します。これは、より速いと、場合によっては、より信頼性のある同等のオフライン技術よりも長いです。インライン型分析技術の数をfとインタフェースされています低原子炉7。例としては、赤外線8,9、紫外可視10,11、NMR 12,13、ラマン分光法14,15、および質量分析法16,17を含みます 。 我々の研究グループは、科学的なマイクロ波ユニット18とラマン分光計をインターフェースしています。これを使用して、反応の範囲は、両方の19定性的および定量的な20の観点から監視されています。この成功を基に、我々は最近、我々の連続フロー単位のいずれかを我々のラマン分光計をインターフェースとキー医薬関連有機変換の数のインライン反応モニタリングのためにそれを採用している。いずれの場合も21には、監視することが可能でした一実施例においても、反応とは、検量線を用いて、我々は、ラマンスペクトルデータからの生成物の変換を決定することができます。ここでは、装置を設定し、反応を監視するためにそれを使用する方法について説明します。我々は3-ACのピペリジン触媒による合成を使用etylcoumarin（1）ここでモデル反応としてアセト酢酸エチル（ 図1）とサリチルアルデヒドから。 <img alt="図1" src="/files/ftp_upload/52393/52393fig1.jpg" /> 図1.ベースが。（1）3-acetylcoumarinを得サリチルアルデヒドとアセト酢酸エチルとの縮合反応を触媒し <a href="https://www.jove.com/files/ftp_upload/52393/52393fig1large.jpg" target="_blank">、この図の拡大版をご覧になるにはこちらをクリックしてください。</a>

<table border="0">
	<tbody>
		<tr>
			<td>Salicylaldehyde</td>
			<td>Sigma-Aldrich</td>
			<td>S356</td>
			<td>Reagent Grade, 98%</td>
		</tr>
		<tr>
			<td>Ethyl acetoacetate</td>
			<td>Acros Organics</td>
			<td>117970010</td>
			<td>99%</td>
		</tr>
		<tr>
			<td>Piperidine</td>
			<td>Sigma-Aldrich</td>
			<td>104094</td>
			<td>Reagent Plus, 99%</td>
		</tr>
		<tr>
			<td>Hydrochloric acid</td>
			<td>Sigma-Aldrich</td>
			<td>320331</td>
			<td>ACS Reagent, 37%</td>
		</tr>
		<tr>
			<td>Ethyl acetate</td>
			<td>Sigma-Aldrich</td>
			<td>34858</td>
			<td>CHROMASOLV, for HPLC, &#62;99.7%</td>
		</tr>
		<tr>
			<td>Acetone</td>
			<td>Sigma-Aldrich</td>
			<td>650501</td>
			<td>CHROMASOLV, for HPLC, &#62;99.9%</td>
		</tr>
		<tr>
			<td>Flow cell</td>
			<td>Starna Cells</td>
			<td></td>
			<td>583.65.65-Q-5/Z20</td>
		</tr>
		<tr>
			<td>Flow unit</td>
			<td>Vapourtec</td>
			<td></td>
			<td>E-series system</td>
		</tr>
		<tr>
			<td>Raman spectrometer</td>
			<td>Enwave Optronics Inc</td>
			<td></td>
			<td>Model EZRaman-L</td>
		</tr>
	</tbody>
</table>

real-time monitoring of reactions performed using continuous-flow processing: the preparation of 3-acetylcoumarin as an example

インラインモニタリングを用いることにより、簡単かつ迅速な方法で、連続フロー処理を​​使用して行われる反応を最適化することができます。これは、この技術を用いて経時的に一貫性のある製品品質を確保することも可能です。ここでは、ラマン分光計で市販のフローユニットを接続する方法を示しています。ラマンフローセルは、それが大気圧で動作させることができることを意味し、背圧調整器の後に配置されています。また、生成物ストリームがフローセルに入る前に管の長さを通過するという事実は、材料が室温であることを意味します。これは、ラマン信号の強度は温度依存性であるので、スペクトルは、等温条件下で取得されることが重要です。装置を組み立てたが、私たちはその後、化学反応をモニターする方法を示し、サリチルアルデヒドとアセト酢酸エチルから3-acetylcoumarinのピペリジン触媒による合成を例として使用されています。反応は、流量の範囲にわたって行うことができるAND温度、 その場の監視ツールは、簡単かつ容易に条件を最適化するために使用されています。

3-acetylcoumarinの連続フロー製造は、インラインモニタリングのための代表的な反応として選ばれました。溶媒として酢酸エチルを使用したときのバッチで、反応が十分に進行します。しかしながら、生成物（1）は、室温で完全に溶解しません。背圧レギュレータの潜在的な目詰まりを防ぐだけでなく、信号取得を乱すことになるフローセル中の固体粒子を持つことのリスクを軽?...

Watch this Scientific Journal Video about Real-time Monitoring of Reactions Performed Using Continuous-flow Processing: The Preparation of 3-Acetylcoumarin as an Example at JoVE.com

Real-time Monitoring of Reactions Performed Using Continuous-flow Processing: The Preparation of 3-Acetylcoumarin as an Example

リアルタイム監視は、連続フロー処理を​​使用して行われる反応の迅速な最適化を可能にします。ここで、3 acetylcoumarinの調製は、例として使用されます。反応を最適化するために必要な手順であるために、その場ラマン監視を行うための装置が記載されています。

連続フロー処理を​​使用して行われる反応のリアルタイムモニタリング：例として3- Acetylcoumarinの調製

By using inline monitoring, it is possible to optimize reactions performed using continuous-flow processing in a simple and rapid way. It is also possible ...

real-time-monitoring-reactions-performed-using-continuous-flow

Research

JoVE Journal

Chemistry

9.6K ビュー.  University of Connecticut. リアルタイム監視は、連続フロー処理を​​使用して行われる反応の迅速な最適化を可能にします。ここで、3 acetylcoumarinの調製は、例として使用されます。反応を最適化するために必要な手順であるために、その場ラマン監視を行うための装置が記載されています。 

ビデオ: Real-time Monitoring of Reactions Performed Using Continuous-flow Processing: The Preparation of 3-Acetylcoumarin as an Example

Rapid High-throughput Species Identification of Botanical Material Using Direct Analysis in Real Time High Resolution Mass Spectrometry

We demonstrate that direct analysis in real time-high resolution mass spectrometry can be used to produce mass spectral profiles of botanical material, and that these chemical fingerprints can be used for plant species identification. The mass spectral data can be acquired rapidly and in a high throughput manner without the need for sample extraction, derivatization or pH adjustment steps. The use of this technique bypasses challenges presented by more conventional techniques including lengthy chromatography analysis times and resource intensive methods. The high throughput capabilities of the direct analysis in real time-high resolution mass spectrometry protocol, coupled with multivariate statistical analysis processing of the data, provide not only class characterization of plants, but also yield species and varietal information. Here, the technique is demonstrated with two psychoactive plant products, Mitragyna speciosa (Kratom) and Datura (Jimsonweed), which were subjected to direct analysis in real time-high resolution mass spectrometry followed by statistical analysis processing of the mass spectral data. The application of these tools in tandem enabled the plant materials to be rapidly identified at the level of variety and species.

A method for species identification of botanical material by direct analysis in real time-high resolution mass spectrometry and multivariate statistical analysis is presented.

リアルタイム高分解能質量分析法で直接分析を用いた植物材料の急速なハイスループット種の同定

We demonstrate that direct analysis in real time-high resolution mass spectrometry can be used to produce mass spectral profiles of botanical material, ...

化学

Capillary Electrophoresis to Monitor Peptide Grafting onto Chitosan Films in Real Time

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. Compared to other analytical separation techniques, such as chromatography, CE is cheap, robust and effectively requires no sample preparation (for a number of complex natural matrices or polymeric samples). CE is fast and can be used to follow the evolution of mixtures in real time (e.g., chemical reaction kinetics), as the signals observed for the separated compounds are directly proportional to their quantity in solution.
Here, the efficiency of CE is demonstrated for monitoring the covalent grafting of peptides onto chitosan films for subsequent biomedical applications. Chitosan&#39;s antimicrobial and biocompatible properties make it an attractive material for biomedical applications such as cell growth substrates. Covalently grafting the peptide RGDS (arginine - glycine - aspartic acid - serine) onto the surface of chitosan films aims at improving cell attachment. Historically, chromatography and amino acid analysis have been used to provide a direct measurement of the amount of grafted peptide. However, the fast separation and absence of sample preparation provided by CE enables equally accurate yet real-time monitoring of the peptide grafting process. CE is able to separate and quantify the different components of the reaction mixture: the (non-grafted) peptide and the chemical coupling agents. In this way the use of CE results in improved films for downstream applications.
The chitosan films were characterized through solid-state NMR (nuclear magnetic resonance) spectroscopy. This technique is more time-consuming and cannot be applied in real time, but yields a direct measurement of the peptide and thus validates the CE technique.

Free solution capillary electrophoresis is a fast, cheap and robust analytical method that enables the quantitative monitoring of chemical reactions in real time. Its utility for rapid, convenient and precise analysis is demonstrated here through analysis of covalent peptide grafting onto chitosan films for improved cell adhesion.

リアルタイムでのキトサンフィルム上にペプチドグラフトを監視するためのキャピラリー電気泳動

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. ...

A Protocol for Safe Lithiation Reactions Using Organolithium Reagents

Organolithium reagents are powerful tools in the synthetic chemist&#39;s toolbox. However, the extreme pyrophoric nature of the most reactive reagents warrants proper technique, thorough training, and proper personal protective equipment. To aid in the training of researchers using organolithium reagents, a thorough, step-by-step protocol for the safe and effective use of tert-butyllithium on an inert gas line or within a glovebox is described. As a model reaction, preparation of lithium tert-butyl amide by the reaction of tert-butyl amine with one equivalent of tert-butyl lithium is presented.

The safe and proper use of organolithium reagents is described.

有機リチウム試薬を用いて安全なリチウム化反応のためのプロトコル

Organolithium reagents are powerful tools in the synthetic chemist&#39;s toolbox. However, the extreme pyrophoric nature of the most reactive reagents ...

Monitoring the Effects of Illumination on the Structure of Conjugated Polymer Gels Using Neutron Scattering

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and absence of white light exposure. By instituting a controlled temperature ramp, the gelation of these materials can be precisely monitored as they proceed through this structural evolution, which effectively mirrors the conditions experienced during the solution deposition phase of organic electronic device fabrication. Using small angle neutron scattering (SANS) and ultra-small angle neutron scattering (USANS) along with appropriate fitting protocols we quantify the evolution of select structural parameters throughout this process. Thorough analysis indicates that continued light exposure throughout the gelation process significantly alters the structure of the ultimately formed gel. Specifically, the aggregation process of poly(3-hexylthiophene-2,5-diyl) (P3HT) nano-scale aggregates is negatively affected by the presence of illumination, ultimately resulting in the retardation of growth in conjugated polymer microstructures and the formation of smaller scale macro-aggregate clusters.

A protocol for the analysis of gels formed from the optoelectronic conjugated polymer poly(3-hexylthiophene-2,5-diyl) (P3HT) using small and ultra-small angle neutron scattering in both the presence and absence of illumination is presented.

中性子散乱法を用いた共役高分子ゲルの構造に対する光照射効果のモニタリング

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and ...

Measurements of Long-range Electronic Correlations During Femtosecond Diffraction Experiments Performed on Nanocrystals of Buckminsterfullerene

The precise details of the interaction of intense X-ray pulses with matter are a topic of intense interest to researchers attempting to interpret the results of femtosecond X-ray free electron laser (XFEL) experiments. An increasing number of experimental observations have shown that although nuclear motion can be negligible, given a short enough incident pulse duration, electronic motion cannot be ignored. The current and widely accepted models assume that although electrons undergo dynamics driven by interaction with the pulse, their motion could largely be considered &#39;random&#39;. This would then allow the supposedly incoherent contribution from the electronic motion to be treated as a continuous background signal and thus ignored. The original aim of our experiment was to precisely measure the change in intensity of individual Bragg peaks, due to X-ray induced electronic damage in a model system, crystalline C60. Contrary to this expectation, we observed that at the highest X-ray intensities, the electron dynamics in C60 were in fact highly correlated, and over sufficiently long distances that the positions of the Bragg reflections are significantly altered. This paper describes in detail the methods and protocols used for these experiments, which were conducted both at the Linac Coherent Light Source (LCLS) and the Australian Synchrotron (AS) as well as the crystallographic approaches used to analyse the data.

We describe an experiment designed to probe the electronic damage induced in nanocrystals of Buckminsterfullerene (C60) by intense, femtosecond pulses of X-rays. The experiment found that, surprisingly, rather than being stochastic, the X-ray induced electron dynamics in C60 are highly correlated, extending over hundreds of unit cells within the crystals1.

バックミンスターフラーレンのナノ結晶のフェムト秒回折実験中長距離電子相関の測定

The precise details of the interaction of intense X-ray pulses with matter are a topic of intense interest to researchers attempting to interpret the ...

Real-time Breath Analysis by Using Secondary Nanoelectrospray Ionization Coupled to High Resolution Mass Spectrometry

Exhaled volatile organic compounds (VOCs) have aroused considerable interest, since they can serve as biomarkers for disease diagnosis and environmental exposure in a non-invasive manner. In this work, we present a protocol to characterize the exhaled VOCs in real time by using secondary nanoelectrospray ionization coupled to high resolution mass spectrometry (Sec-nanoESI-HRMS). The homemade Sec-nanoESI source was readily set up based on a commercial nanoESI source. Hundreds of peaks were observed in the background-subtracted mass spectra of exhaled breath, and the mass accuracy values are -4.0-13.5 ppm and -20.3-1.3 ppm in the positive and negative ion detection modes, respectively. The peaks were assigned with accurate elemental composition according to the accurate mass and isotopic pattern. Less than 30 s is used for one exhalation measurement, and it takes approximately 7 min for six replicated measurements.

A protocol for characterizing chemical composition of exhaled breath in real time by using secondary nanoelectrospray ionization coupled to high resolution mass spectrometry is demonstrated.

高分解能質量分析に結合された二次 Nanoelectrospray イオン化を用いたリアルタイム呼吸解析

Exhaled volatile organic compounds (VOCs) have aroused considerable interest, since they can serve as biomarkers for disease diagnosis and environmental ...

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.

P- ニトロ安息香酸の存在の連続流れ化学: 反作用

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

A Continuous-flow Photocatalytic Reactor for the Precisely Controlled Deposition of Metallic Nanoparticles

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic nanoparticles is developed. Guidelines for the replication of the reactor and its operation are provided in detail. Three different composite systems (Pt/graphene, Pt/TiO2, and Au/TiO2) with monodisperse and uniformly distributed particles are produced by this reactor, and the photodeposition mechanism, as well as the synthesis optimization strategy, are discussed. The synthesis methods and their technical aspects are described comprehensively. The role of the ultraviolet (UV) dose (in each excitation pulse) on the photodeposition process is investigated and the optimum values for each composite system are provided.

For a continuous and scalable synthesis of noble-metal-based nanocomposites, a novel photocatalytic reactor is developed and its structure, operation principles, and product quality optimization strategies are described.

金属ナノ粒子の正確に制御された沈着量の連続的な流れの光触媒反応

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic ...

Technical Aspect of the Automated Synthesis and Real-Time Kinetic Evaluation of [11C]SNAP-7941

Positron emission tomography (PET) is an essential molecular imaging technique providing insights into pathways and using specific targeted radioligands for in vivo investigations. Within this protocol, a robust and reliable remote-controlled radiosynthesis of [11C]SNAP-7941, an antagonist to the melanin-concentrating hormone receptor 1, is described. The radiosynthesis starts with cyclotron produced [11C]CO2 that is subsequently further reacted via a gas-phase transition to [11C]CH3OTf. Then, this reactive intermediate is introduced to the precursor solution and forms the respective radiotracer. Chemical as well as the radiochemical purity are determined by means of RP-HPLC, routinely implemented in the radiopharmaceutical quality control process. Additionally, the molar activity is calculated as it is a necessity for the following real-time kinetic investigations. Furthermore, [11C]SNAP-7941 is applied to MDCKII-WT and MDCKII-hMDR1 cells for evaluating the impact of P-glycoprotein (P-gp) expression on cell accumulation. For this reason, the P-gp expressing cell line (MDCKII-hMDR1) is either used without or with blocking prior to experiments by means of the P-gp substrate (&#177;)-verapamil and the results are compared to the ones observed for the wildtype cells. The overall experimental approach demonstrates the importance of a precise time-management that is essential for every preclinical and clinical study using PET tracers radiolabelled with short-lived nuclides, such as carbon-11 (half-life: 20 min).

Technical Aspect of the Automated Synthesis and Real-Time Kinetic Evaluation of [11C]SNAP-7941

Here, we represent a protocol for the fully automated radiolabelling of [11C]SNAP-7941 and the analysis of the real-time kinetics of this PET-tracer on P-gp expressing and non-expressing cells.

[11C]SNAP-7941の自動合成とリアルタイム運動評価の技術的側面

Positron emission tomography (PET) is an essential molecular imaging technique providing insights into pathways and using specific targeted radioligands ...

Optimization of Radiochemical Reactions using Droplet Arrays

Current automated radiosynthesizers are designed to produce large clinical batches of radiopharmaceuticals. They are not well suited for reaction optimization or novel radiopharmaceutical development since each data point involves significant reagent consumption, and contamination of the apparatus requires time for radioactive decay before the next use. To address these limitations, a platform for performing arrays of miniature droplet-based reactions in parallel, each confined within a surface-tension trap on a patterned polytetrafluoroethylene-coated silicon "chip", was developed. These chips enable rapid and convenient studies of reaction parameters including reagent concentrations, reaction solvent, reaction temperature and time. This platform permits the completion of hundreds of reactions in a few days with minimal reagent consumption, instead of taking months using a conventional radiosynthesizer.

This method describes the use of a novel high-throughput methodology, based on droplet chemical reactions, for the rapid and economical optimization of radiopharmaceuticals using nanomole amounts of reagents.

連続フロー処理を​​使用して行われる反応のリアルタイムモニタリング：例として3- Acetylcoumarinの調製

連続フロー処理を使用して行われる反応のリアルタイムモニタリング：例として3- Acetylcoumarinの調製