この作品は、バージニア工科大学と州立大学からスタートアップの資金によって支えられました。Q.F. は、国家自然科学基金、中国の (21504047)、江蘇省の自然科学財団 (BK20150834)、南京大学の記事および通信科学財団 NUPTSF (NY214179) からの支援を認めています。

注意: は、すべて関連材料の安全データ用紙 (MSDS) 使用する前にご相談ください。合成で使用されている多くの化学物質、急性毒性、発癌性。反応工学的制御 (ヒューム フードとグローブ ボックス) と個人用保護具 (保護メガネ、手袋、白衣、フルレングスのパンツ、閉じてつま先の靴、青の光の使用を含むを実行するときにすべての適切な安全対策を使用してください。ブロック安全ゴーグル)。次の手順は、グローブ ボックスの標準的な無料の空気処理技術を含みます。すべてのソリューションは、ピペットを使用して転送されます。
1. 触媒との発信側の準備
注: 全体のプロセスは、コールド トラップをグローブ ボックスで実施します。すべての化学物質は乾燥またはボックスに移動する前に精製します。13すべてのバイアルとガラス乾燥させ、ボックスに移動する前に、オーブンで加熱します。
<ol><li>
(Bpy)Ni(COD) 溶液の調製 注: (bpy)Ni(COD) たておかなければ、その場で。それはグローブ ボックス冷凍庫 (-35 ° C) に格納されている必要があります、1 週間以内に使用します。他のすべての触媒およびイニシエーター ソリューションに格納できるグローブ ボックス冷凍庫 1 ヶ月以上。<ol>
<li>7 mL シンチレーション バイアルに Ni(COD)2 (3.5 mg、12.7 µmol 1.0 eq) を考慮します。</li>
		<li>2, 2 '-ビピリジン (5.9 mg、37.8 µmol) 7 mL シンチレーション バイアルに重量を量る。</li>
		<li>2, 2 '-ビピリジンを 1 mL の無水テトラヒドロ フラン (THF) を解散します。</li>
		<li>結果として得られる 2, 2 '-ビピリジン ソリューション (337 μ L) Ni(COD)2バイアルを追加します。</li>
		<li>1 mL の無水 thf に混合物を希釈します。</li>
		<li>バイアルのキャップ、2 時間室温で反応混合物を配置します。 注: Ni(COD)2は THF に溶解しないに対し (bpy)Ni(COD) THF に溶解。紫のソリューションで 2 時間後沈殿物はないはずです。</li>
		<li>ストア (-35 ° C のフリーザーで bpy)Ni(COD)。</li>
	</ol>
</li>
	<li>
Zn(HMDS)2溶液の調製
	<ol>
<li>7 mL シンチレーション バイアルに Zn(HMDS)2 (3.3 mg、4 μ L、8.5 µmol) を追加します。</li>
		<li>Zn(HMDS)2 1 mL の無水 thf に溶解します。</li>
		<li>-35 ° C のフリーザーに Zn(HMDS)2ソリューションを格納します。</li>
	</ol>
</li>
	<li>
BnOH 溶液の調製
	<ol>
<li>7 mL シンチレーション バイアルに BnOH (4.0 mg、4 μ L、37.0 µmol) を追加します。</li>
		<li>BnOH 4 mL の無水 thf に溶解します。</li>
		<li>-35 ° C のフリーザーに BnOH ソリューションを格納します。</li>
	</ol>
</li>
	<li>
Ir 1 溶液の調製
	<ol>
<li>グローブ ボックス ライトをオフにします。 注意: それは重合前にIr 1の非アクティブ化を避けるためにグローブ ボックス ライトをオフにする必要は。</li>
		<li>7 mL シンチレーション バイアルにIr 1 (2.9 mg, 2.6 µmol) を追加します。</li>
		<li>Ir 1 3 mL の無水 thf に溶解します。</li>
		<li>-35 ° C のフリーザーでIr 1ソリューションを格納します。</li>
	</ol>
</li>
</ol>2. l-1 のユウロピウム開環重合
注: 全体のプロセスは、コールド トラップをグローブ ボックスで実施します。すべての OCA モノマーは、使用する前にグローブ ボックスに再結晶しました。13 DP で重合の例を与える私たちここで 500 を = ([l -1]/[(bpy)Ni(COD)]/[Zn(HMDS)2]/[BnOH]/[Ir 1] = 500/1/1/1/0.1)。異なる DPs でポリマーはモノマーを質量に応じて調整することによっても用意できます。
<ol><li>
重合用 l-1 溶液の調製
	<ol>
<li>7 mL シンチレーション バイアルに l-1 (72.2 mg, 375.7 µmol) を追加します。</li>
		<li>無水 thf 722 μ L に l-1を溶解します。</li>
		<li>攪拌棒装備別のシンチレーション 7 mL バイアルに l-1溶液 200 μ L を追加します。</li>
		<li>7 mL シンチレーション バイアルに無水 thf 中の 100 μ L を追加します。</li>
		<li>バイアルのキャップし、コールド トラップの l-1ソリューションを配置します。</li>
		<li>グローブ ボックス ライトをオフにします。 注意: それは重合前にIr 1の非アクティブ化を避けるためにグローブ ボックス ライトをオフにする必要は。</li>
	</ol>
</li>
	<li>
コールド トラップを冷却
	<ol>
<li>箱の中には、コールド トラップに温度計を入れます。</li>
		<li>ボックスの外側を追加 ca。 500 mL のエタノールのデュワー フラスコ。</li>
		<li>デュワー フラスコに液体窒素を追加します。</li>
		<li>コールド トラップに KGW デュワー フラスコをロードします。</li>
		<li>-50 ° c. にコールド トラップを冷却します。</li>
		<li>入れてかき混ぜるプレート下、コールド トラップ (図 1参照)。</li>
	</ol>
</li>
	<li>
ユウロピウム開環重合を実行します。 注: 重合を開始する前に場所の安全ブロックを青い光が届くゴーグルします。すべての触媒システム ソリューションをすぐに冷凍庫から取り出して 20 mg l-1一時停止または中断なしの 30 以上を含む 7 mL シンチレーション バイアルに順次付加 s。<ol>
<li>ソリューションを追加 (bpy)Ni(COD) (16.4 μ L、0.208 µmol) l-1 (2.1 の準備) バイアル 7 mL シンチレーションに。</li>
		<li>バイアルに Zn(HMDS)2ソリューション (24.4 μ L、0.208 µmol) を追加します。</li>
		<li>バイアルに BnOH 溶液 (22.5 μ L、0.208 µmol) を追加します。</li>
		<li>バイアルに Ir 1 ソリューション (24.2 μ L, 0.0208 µmol) を追加し、バイアルのキャップします。</li>
		<li>青の LED 光を遮断、安全ゴーグルを着用します。 注意: 相対高強度の光を使用して青色 LED として、全体のプロセスの中に安全ゴーグルを着用します。</li>
		<li>光青 LED ライト (34 W) と LED によって生成される熱を放散するファンを入れます。コールド トラップのバイアルに光を向けます。(図 1)</li>
		<li>かくはんを入れます。</li>
		<li>アルミ箔コールド トラップをカバーします。</li>
		<li>-15 ± 5 ° C で反応温度を維持し、15-20 分ごと液体窒素を追加します。 注: 反応温度の維持は、重合の MW が重要です。</li>
	</ol>
</li>
</ol>3. モニター モノマー変換フーリエ変換赤外吸収スペクトル
注: フーリエ変換赤外吸収スペクトル (FTIR) ダイヤモンド ATR と伝送サンプリング アクセサリ装備 FT-IR 分光器に記録されます。
<ol><li>特定の時点で 7 mL シンチレーション バイアルに高分子溶液 (20 μ L) の小さい因数を追加し、頂いた。</li>
	<li>グローブ ボックスのバイアルを削除します。</li>
	<li>赤外 ATR ダイヤモンド サンプラーにソリューション (3 μ L) をすぐにドロップします。ソリューション フォーム 10 内映画スペクトル測定のための s。</li>
	<li>試料の赤外スペクトルを測定します。 注: モノマー変換された 1760 cm-1と 1805s cm-1の間強度比によって決定されます: 変換 % =1760/(私1760 +1805) (代表は、図 2の結果)。一般的に、重合は、1 8 h 約 200 から 1000 まで DP (詳細な動態は参照13で説明します)。</li>
</ol>4. ゲル浸透クロマトグラフィーによる高分子の分子量の測定
注: ゲル浸透クロマトグラフィー (GPC) 実験は、脱ガス装置、システム レーザー光散乱 (MALS) 検出器搭載者のイソクラティック ポンプ システムで実行されます (GaAs 30 mW レーザー λ = 690 nm)、および差動屈折 (DRI) 検出器690 nm の光源。直列サイズ排除カラムを使用して色分解を実行 (100 Å、500 Å、103 Å と 104 Å 列、5 μ m、300 × 4.6 mm) 35 ° c a 0.35 mL/min の流速で移動相として THF を使用します。ポリマーの分子量 (MW) と分子量分布 (Ð) は、MALS DRI データの適合 Zimm 模型を使用して決定されます。金属、高分子錯体の存在は、GPC 測定結果には影響しません。
<ol><li>グローブ ボックスの高分子溶液 (50 μ L) の小さい因数を削除します。</li>
	<li>バイアルに thf 100 μ L を追加します。</li>
	<li>GPC サンプラーにサンプルを注入します。</li>
	<li>GPC の実行が完了したら、結果を分析します。 注: ポリマーは、狭いĐと単分散をする必要があります (図 3の結果代表)。ポリマー (20 mg) を乾燥し、Ni の 87%、亜鉛錯体、誘導結合プラズマ質量分析法 (ICP-MS) による決定の 50% を削除することができます 1% とし、1 mL メタノール含有 1 mL ジエチル エーテルで洗浄することができます。</li>
</ol>

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Lett. 7, 1169-1172 (2005).</li><li>Yin, Q., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Drug-initiated+ring-opening+polymerization+of+O-carboxyanhydrides+for+the+preparation+of+anticancer+drug-poly(O-carboxyanhydride)+nanoconjugates.">Drug-initiated ring-opening polymerization of O-carboxyanhydrides for the preparation of anticancer drug-poly(O-carboxyanhydride) nanoconjugates.</a> Biomacromolecules. 14, 920-929 (2013).</li></ol>

著者は競合する金銭的な利益を宣言しません。仮特許 (米国特許アプリケーションなし: 62/414,016) 本稿で示された結果に係る提出されています。

-15 ± 反応温度を維持しているプロトコルの中で重要なステップ 5 ° Cすべての触媒ソリューションおよび OCA モノマー重合前に-35 ° C でグローブ ボックスの冷凍庫で保存する必要。反応容器は、コールド トラップで予冷する必要があります。LED ライト放散熱のため、反応中に 15-20 分ごとの反応を監視する必要は。温度を上げて一度を追加とする-10 ° C、液体窒素デュワー トラップを冷却す?...

ポリ (α-ヒドロキシ酸) (ケヤパハ) バイオメディカル機器から包装に至るまでのアプリケーションと生分解性、生体適合性ポリマーの重要なクラスであります。1,2が PAHAs α-ヒドロキシ酸の重縮合による直接準備することができます、結果の PAHAs の分子量 (MWs) は一般的に低い。3 (例えば、乳酸とグリコール酸) ラクトンの開環重合 (ROP) 重縮合より MWs と分子量分布 (Đ) のよりよい制御を提供する合成手法であります。ただし、PAHAs とラクトンの側鎖の機能の欠如は、物理・化学的性質とその応用の多様性を制限します。4,5 、2006 年から 1, 3-dioxolane-2, 4-diones、いわゆるO- carboxyanhydrides (OCAs)、側鎖の機能の豊富な6,7,8,と準備することができます9,10,11,12,13は、ポリエステルの重合用高活性モノマーの代替クラスとして浮上しています。14,15
OCAs ROP の触媒システムは、触媒、8,12,16,17有機金属触媒12,18,19 に分類できます。、20,21と生体触媒。22一般に、触媒によって促進される OCAs ROP は OCAs 電子グループ、8,17を軸受のエピマー化 (すなわち、年の欠如) などのもっとまたはより少なく自由な方法で進む予測不可能な MWs または遅い重合速度論。13これらの問題に対処するため作業中の Zn アルコキシド コンプレックスは OCAs ROP のため開発されました。12マテリアルインテグレーション Rop は、重合度の低い (DP) エピマー化なしで達成されました。ただし、この亜鉛アルコキシドの触媒は効率的に重合 (DP ≥ 300) の高度でポリマーを生成できません。13
我々 は最近、カスタマイズ性とケヤパハ合成 (図 1) の効率を大幅に向上させる有望なアプローチを報告しています。13 OCAs の開環重合を仲介する亜鉛アルコキシドと OCA の脱炭酸を促進するユウロピウム Ni/Ir 触媒をマージします。低温 (-15 ° C) およびユウロピウム Ni/Ir 触媒の使用は相乗的開環し、OCA の望ましくない副反応を回避しながらチェーン伝播 Ni カルボニルの形成などの脱炭酸を加速します。23,24 ni 複雑なトランス メタル化にアクティブな Zn アルコキシドはチェーン伝達の鎖末端にあります。13
このプロトコルでは、新鮮な準備追加 (bpy)Ni(COD) (bpy = 2, 2'-ビピリジル、タラ = 1, 5-シクロオクタジエン)、Zn(HMDS)2 (HMDS = ヘキサメチルジシラザン)、25ベンジル アルコール (BnOH) と Ir [dF (CF3) ppy]2(dtbbpy) PF6 (Ir 1dF (CF3) ppy = 2-(2, 4-difluorophenyl)-5-(トリフルオロメチル) ピリジン、dtbbpy = 4, 4' - ジ-tert- ブチル-2, 2'-ビピリジン) の存在下でのコールド トラップ付きグローブ ボックスでモノマーの l-1ソリューション26に、ブルーの LED ライト (400-500 nm) と温度 (図 1) を維持するためにファンが。温度は-15 ° C ± 5 ° C で重合中に保持されます。OCA の変換は、フーリエ変換赤外分光法によって監視されます。得られたポリマー MWs とĐs は、ゲル浸透クロマトグラフィー (GPC) によって特徴付けられます。Homodecoupling 1H nmr による研究は、得られるポリマーがアイソタク チックであるかどうかを決定します。ほとんどの化学薬品は水分に非常に敏感、詳しいビデオ プロトコル落とし穴ユウロピウム OCAs ROP に関連付けられている新しい実務を支援するものです。

<table>
	<tbody>
		<tr>
			<td>Ni(COD)2</td>
			<td>Strem</td>
			<td>28-0010</td>
			<td>Stored in the glove box freezer.</td>
		</tr>
		<tr>
			<td>2,2&#8242;-bipyridine</td>
			<td>Strem</td>
			<td>07-0290</td>
			<td>Stored in the glove box freezer.</td>
		</tr>
		<tr>
			<td>Zn(HMDS)2</td>
			<td>N/A</td>
			<td>N/A</td>
			<td>Synthesized following reported procedures.25 Stored in the glove box freezer.</td>
		</tr>
		<tr>
			<td>Benzyl alcohol</td>
			<td>Sigma-Aldrich</td>
			<td>402834</td>
			<td>Stored with 4&#197; molecular sieve</td>
		</tr>
		<tr>
			<td>Ir[dF(CF3)ppy]2(dtbbpy)PF6</td>
			<td>Strem</td>
			<td>77-0425</td>
			<td>Stored in the glove box freezer.</td>
		</tr>
		<tr>
			<td>THF</td>
			<td>Sigma-Aldrich</td>
			<td>34865</td>
			<td>Dried by alumina columns and stored with 4&#197; molecular sieve in the dark bottle in the glove box.</td>
		</tr>
		<tr>
			<td>Ethanol</td>
			<td>Sigma-Aldrich</td>
			<td>793175</td>
			<td></td>
		</tr>
		<tr>
			<td>GPC with an isocratic pump</td>
			<td>Agilent</td>
			<td>Agilent 1260 series</td>
			<td></td>
		</tr>
		<tr>
			<td>Dawn Heleos II Light Scatterer</td>
			<td>Wyatt</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Optilab rEX differential refractive index detector</td>
			<td>Wyatt</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Size exclusion columns</td>
			<td>Phenomenex</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Glass Scintillation Vials - 7 ml</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>FTIR spectrometer</td>
			<td>Agilent</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Stir bars</td>
			<td>VWR</td>
			<td>58948-091</td>
			<td></td>
		</tr>
		<tr>
			<td>Balance</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Glove box</td>
			<td>Mbraun</td>
			<td>Labstar Pro</td>
			<td></td>
		</tr>
	</tbody>
</table>

controlled photoredox ring-opening polymerization of o-carboxyanhydrides mediated by ni/zn complexes

ここでは、予想される分子量 Zn アルコキシドのアイソタク チック ポリ (α-ヒドロキシ酸) の合成を可能にする効率的な開環重合用の Ni/Ir 触媒を組み合わせた効果的なプロトコルについて述べる (> 140kDa) と分子量分布の狭い (Mw/Mn < 1.1)。この開環重合は、アルコール イニシエーターと青色 LED (400-500 nm) 照射ユウロピウム Ir 触媒存在下での Ni と Zn の複合体によって媒介されます。重合は、望ましくない副反応を避けるために低温 (-15 ° C) で行われます。完全なモノマーの消費は、狭い分子量分布を持つ期待の分子量に近い高分子を提供 4-8 時間以内実現できます。結果数平均分子量 1000 まで重合度と相関を示しています。Homodecoupling 1H nmr による研究は、得られたポリマーはエピマー化せずアイソタク チックであることを確認します。この重合を本報告では、立体規則ポリ (α-ヒドロキシ酸) やその共重合体の様々 な機能的な側鎖グループを軸受を準備する急速な制御のO- carboxyanhydrides 重合を達成するための戦略を提供しています。

図 2に示すように、OCA の変換はフーリエ変換赤外分光法によって監視されます。OCA の無水結合ストレッチとして 1805 cm-1にピークが割り当てられます1760 cm-1にピークは、ポリマー中のエステル結合の形成に対応します。1805 cm-1にモノマーのピークが完全に消えると、重合が完了します。
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Watch this Scientific Journal Video about Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes at JoVE.com

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

Ocarboxyanhydrides ニッケル/亜鉛錯体による媒介の制御されたユウロピウム開環重合用プロトコルである. します。

OCarboxyanhydrides ニッケル/亜鉛錯体による媒介のユウロピウムの開環重合

Here, we describe an effective protocol that combines photoredox Ni/Ir catalysis with the use of a Zn-alkoxide for efficient ring-opening polymerization, ...

controlled-photoredox-ring-opening-polymerization-o-carboxyanhydrides

Research

JoVE Journal

Chemistry

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

8.0K ビュー.  Nanjing University of Posts and Telecommunications. Ocarboxyanhydrides ニッケル/亜鉛錯体による媒介の制御されたユウロピウム開環重合用プロトコルである. します。

ビデオ: Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

Production of Disulfide-stabilized Transmembrane Peptide Complexes for Structural Studies

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

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

構造研究のためのジスルフィド安定化膜貫通ペプチド複合体の生産

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

化学

Anticancer Metal Complexes: Synthesis and Cytotoxicity Evaluation by the MTT Assay

Titanium (IV) and vanadium (V) complexes are highly potent anticancer agents. A challenge in their synthesis refers to their hydrolytic instability; therefore their preparation should be conducted under an inert atmosphere. Evaluation of the anticancer activity of these complexes can be achieved by the MTT assay.
The MTT assay is a colorimetric viability assay based on enzymatic reduction of the MTT molecule to formazan when it is exposed to viable cells. The outcome of the reduction is a color change of the MTT molecule. Absorbance measurements relative to a control determine the percentage of remaining viable cancer cells following their treatment with varying concentrations of a tested compound, which is translated to the compound anticancer activity and its IC50 values. The MTT assay is widely common in cytotoxicity studies due to its accuracy, rapidity, and relative simplicity.
Herein we present a detailed protocol for the synthesis of air sensitive metal based drugs and cell viability measurements, including preparation of the cell plates, incubation of the compounds with the cells, viability measurements using the MTT assay, and determination of IC50 values.

A method for synthesis of air-sensitive titanium and vanadium anticancer agents is described, along with the evaluation of their cytotoxic activity towards human cancer cell line by the MTT Assay.

MTTアッセイにより合成と細胞毒性の評価：抗がん金属錯体

Titanium (IV) and vanadium (V) complexes are highly potent anticancer agents. A challenge in their synthesis refers to their hydrolytic instability; ...

Facile and Efficient Preparation of Tri-component Fluorescent Glycopolymers via RAFT-controlled Polymerization

Synthetic glycopolymers are instrumental and versatile tools used in various biochemical and biomedical research fields. An example of a facile and efficient synthesis of well-controlled fluorescent statistical glycopolymers using reversible addition-fragmentation chain-transfer (RAFT)-based polymerization is demonstrated. The synthesis starts with the preparation of &#946;-galactose-containing glycomonomer 2-lactobionamidoethyl methacrylamide obtained by reaction of lactobionolactone and N-(2-aminoethyl) methacrylamide (AEMA). 2-Gluconamidoethyl methacrylamide (GAEMA) is used as a structural analog lacking a terminal &#946;-galactoside. The following RAFT-mediated copolymerization reaction involves three different monomers: N-(2-hydroxyethyl) acrylamide as spacer, AEMA as target for further fluorescence labeling, and the glycomonomers. Tolerant of aqueous systems, the RAFT agent used in the reaction is (4-cyanopentanoic acid)-4-dithiobenzoate. Low dispersities (&#8804;1.32), predictable copolymer compositions, and high reproducibility of the polymerizations were observed among the products. Fluorescent polymers are obtained by modifying the glycopolymers with carboxyfluorescein succinimidyl ester targeting the primary amine functional groups on AEMA. Lectin-binding specificities of the resulting glycopolymers are verified by testing with corresponding agarose beads coated with specific glycoepitope recognizing lectins. Because of the ease of the synthesis, the tight control of the product compositions and the good reproducibility of the reaction, this protocol can be translated towards preparation of other RAFT-based glycopolymers with specific structures and compositions, as desired.

An efficient, three-step synthesis of RAFT-based fluorescent glycopolymers, consisting of glycomonomer preparation, copolymerization, and post-modification, is demonstrated. This protocol can be used to prepare RAFT-based statistical glycopolymers with desired structures.

RAFT制御重合によるトライ成分蛍光グリコの容易かつ効率的な準備

Synthetic glycopolymers are instrumental and versatile tools used in various biochemical and biomedical research fields. An example of a facile and ...

Ethylene Polymerizations Using Parallel Pressure Reactors and a Kinetic Analysis of Chain Transfer Polymerization

We demonstrate a method for high-throughput catalyst screening using a parallel pressure reactor starting from the initial synthesis of a nickel &#945;-diimine ethylene polymerization catalyst. Initial polymerizations with the catalyst lead to optimized reaction conditions, including catalyst concentration, ethylene pressure and reaction time. Using gas-uptake data for these reactions, a procedure to calculate the initial rate of propagation (kp) is presented. Using the optimized conditions, the ability of the nickel &#945;-diimine polymerization catalyst to undergo chain transfer with diethylzinc (ZnEt2) during ethylene polymerization was investigated. A procedure to assess the ability of the catalyst to undergo chain transfer (from molecular weight and 13C NMR data), calculate the degree of chain transfer, and calculate chain transfer rates (ke) is presented.

A protocol for the high-throughput analysis of polymerization catalyst, chain transfer polymerizations, polyethylene characterization, and reaction kinetic analysis is presented.

並列圧力反応器および連鎖移動重合の速度論的解析を使用してエチレン重合

We demonstrate a method for high-throughput catalyst screening using a parallel pressure reactor starting from the initial synthesis of a nickel ...

Atom Transfer Radical Polymerization of Functionalized Vinyl Monomers Using Perylene as a Visible Light Photocatalyst

A standardized technique for atom transfer radical polymerization of vinyl monomers using perylene as a visible-light photocatalyst is presented. The procedure is performed under an inert atmosphere using air- and water-exclusion techniques. The outcome of the polymerization is affected by the ratios of monomer, initiator, and catalyst used as well as the reaction concentration, solvent, and nature of the light source. Temporal control over the polymerization can be exercised by turning the visible light source off and on. Low dispersities of the resultant polymers as well as the ability to chain-extend to form block copolymers suggest control over the polymerization, while chain end-group analysis provides evidence supporting an atom-transfer radical polymerization mechanism.

A method for the atom transfer radical polymerization of functionalized vinyl monomers using perylene as a visible-light photocatalyst is described.

可視光応答型光触媒としてペリレンを使用した官能ビニルモノマーの原子移動ラジカル重合

A standardized technique for atom transfer radical polymerization of vinyl monomers using perylene as a visible-light photocatalyst is presented. The ...

Facile Synthesis of Worm-like Micelles by Visible Light Mediated Dispersion Polymerization Using Photoredox Catalyst

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins with the synthesis of a hydrophilic poly(oligo(ethylene glycol) methyl ether methacrylate) (POEGMA) homopolymer using reversible addition-fragmentation chain-transfer (RAFT) polymerization. Under mild visible light irradiation (&#955; = 460 nm, 0.7 mW/cm2), this macro-chain transfer agent (macro-CTA) in the presence of a ruthenium based photoredox catalyst, Ru(bpy)3Cl2 can be chain extended with a second monomer to form a well-defined block copolymer in a process known as Photoinduced Electron Transfer RAFT (PET-RAFT). When PET-RAFT is used to chain extend POEGMA with benzyl methacrylate (BzMA) in ethanol (EtOH), polymeric nanoparticles with different morphologies are formed in situ according to a polymerization-induced self-assembly (PISA) mechanism. Self-assembly into nanoparticles presenting POEGMA chains at the corona and poly(benzyl methacrylate) (PBzMA) chains in the core occurs in situ due to the growing insolubility of the PBzMA block in ethanol. Interestingly, the formation of highly pure worm-like micelles can be readily monitored by observing the onset of a highly viscous gel in situ due to nanoparticle entanglements occurring during the polymerization. This process thereby allows for a more reproducible synthesis of worm-like micelles simply by monitoring the solution viscosity during the course of the polymerization. In addition, the light stimulus can be intermittently applied in an ON/OFF manner demonstrating temporal control over the nanoparticle morphology.

This article describes a process for producing polymeric self-assembled nanoparticles using visible light mediated dispersion polymerization. Using low energy visible light to control the polymerization allows for the reproducible formation of self-assembled worm-like micelles at high solids content.

Photoredox触媒を用いた可視光媒介分散重合によるワームのようなミセルの簡便な合成

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins ...

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &#960;-&#960; Stacking Interactions

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE). Characterization of the copolymer revealed a narrow molecular distribution (PDI &#60; 1.03) and confirmed the degree of polymerization of mPEG122-b-(PheGE)15. The critical micelle concentration of the copolymer was evaluated using an established fluorescence method with the aggregation behavior evaluated by dynamic light scattering and transmission electronic microscopy. The potential of the copolymer for use in drug delivery applications was evaluated in a preliminary manner including in vitro biocompatibility, loading and release of the hydrophobic anti-cancer drug doxorubicin (DOX). A stable micelle formulation of DOX was prepared with drug loading levels up to 14% (wt%), drug loading efficiencies &#62; 60% (w/w) and sustained release of drug over 4 days under physiologically relevant conditions (acidic and neutral pH, presence of albumin). The high drug loading level and sustained release is attributed to stabilizing &#960;-&#960; interactions between DOX and the core-forming block of the micelles.

The key steps of living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE) are described. The resulting block copolymer micelles (BCMs) were loaded with doxorubicin 14% (wt%) and sustained release of drug over 4 days under physiologically relevant conditions was obtained.

π-πスタッキング相互作用によって安定化されたブロック共重合体ミセルの調製のための両親媒性共重合体のアニオン重合

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl ...

A Simple and Efficient Protocol for the Catalytic Insertion Polymerization of Functional Norbornenes

Norbornene can be polymerized by a variety of mechanisms, including insertion polymerization whereby the double bond is polymerized and the bicyclic nature of the monomer is conserved. The resulting polymer, polynorbornene, has a very high glass transition temperature, Tg, and interesting optical and electrical properties. However, the polymerization of functional norbornenes by this mechanism is complicated by the fact that the endo substituted norbornene monomer has, in general, a very low reactivity. Furthermore, the separation of the endo substituted monomer from the exo monomer is a tedious task. Here, we present a simple protocol for the polymerization of substituted norbornenes (endo:exo ca. 80:20) bearing either a carboxylic acid or a pendant double bond. The process does not require that both isomers be separated, and proceeds with low catalyst loadings (0.01 to 0.02 mol%). The polymer bearing pendant double bonds can be further transformed in high yield, to afford a polymer bearing pendant epoxy groups. These simple procedures can be applied to prepare polynorbornenes with a variety of functional groups, such as esters, alcohols, imides, double bonds, carboxylic acids, bromo-alkyls, aldehydes and anhydrides.

We describe the catalytic insertion polymerization of 5-norbornene-2-carboxylic acid and 5-vinyl-2-norbornene to form functional polymers with a very high glass transition temperature.

機能性ノルボルネンの触媒挿入重合のためのシンプルで効率的なプロトコル

Norbornene can be polymerized by a variety of mechanisms, including insertion polymerization whereby the double bond is polymerized and the bicyclic ...

Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source

This protocol demonstrates a method for ramie fiber extraction by scouring raw ramie in an alkali hydrogen peroxide system supported by a controlled-release alkali source. The fiber extracted from ramie is a type of textile material of great importance. In previous studies, ramie fiber was extracted in an alkali hydrogen peroxide system supported only by sodium hydroxide.However, due to the strong alkalinity of sodium hydroxide, the oxidation reaction speed of hydrogen peroxide was difficult to control and thus resulted in great damage to the treated fiber. In this protocol, a controlled-release alkali source, which is composed of sodium hydroxide and magnesium hydroxide, is used to provide an alkali condition and buffer the pH value of the alkali hydrogen peroxidesystem. The substitution rate of magnesium hydroxide can adjust the pH value of the hydrogen peroxide system and has great influence on the fiber properties. The pH value and oxidation-reduction potential (ORP) value, which represents the oxidation ability of alkali hydrogen peroxide system, were monitored using a pH meter and ORP meter, respectively. The residual hydrogen peroxide content in the alkali hydrogen peroxide system during the extraction process and the chemical oxygen demand (COD) value of wastewater after fiber extraction are tested by KMnO4 titration method. The yield of fiber is measured using a precision electronic balance, and residual gums of fiber are tested by a chemical analysis method. The polymerization degree (PD value) of fiber is tested by an intrinsic viscosity method using the Ubbelohde viscometer. The tensile property of fiber, including tenacity, elongation, and rupture, is measured using a fiber strength instrument. Fourier transform infrared spectroscopy and X-ray diffraction are used to characterize the functional groups and crystal property of fiber. This protocol proves that the controlled-release alkali source can improve the properties of the fiber extracted in an alkali hydrogen peroxide system.

Presented here is a protocol for extraction of ramie fiber in alkali hydrogen peroxide system supported by controlled-release alkali source.

アルカリ過酸化水素システム制御リリース アルカリ ソースによってサポートされるラミー繊維の抽出

This protocol demonstrates a method for ramie fiber extraction by scouring raw ramie in an alkali hydrogen peroxide system supported by a ...

Preparation of Hollow Polystyrene Particles and Microcapsules by Radical Polymerization of Janus Droplets Consisting of Hydrocarbon and Fluorocarbon Oils

In this article, we have demonstrated a method for producing hollow particles and microcapsules using oil droplets consisting of hydrocarbon oil (styrene) and fluorocarbon oil (perfluoro-n-octane, PFO) in aqueous surfactant (sodium dodecylsulfate, SDS) solutions. Since fluorocarbon oils are immiscible with hydrocarbon oils, the two oils are separated. Emulsions are prepared by stirring styrene/PFO/aqueous SDS solution mixtures at 80 &#176;C. The type of emulsions and the morphology of droplets in the emulsions are observed by light microscope and scanning confocal fluorescence microscope. It is found that oil droplets with Janus-type morphologies consisting of mutually immiscible styrene and PFO are formed in aqueous SDS solutions. Polystyrene particles are fabricated by radical polymerization of the ternary mixtures of styrene/PFO/aqueous SDS solution at 80 &#176;C. The morphologies of the polystyrene are confirmed by scanning electron microscopy and scanning transmission electron microscopy observations. These observations show the preparation of hollow polystyrene particles with a single hole on the surface. To our knowledge, this method is a novel strategy using the immiscibility of hydrocarbon and fluorocarbon oils. The hollow particles can also be applied to the preparation of microcapsules.

A protocol for the fabrication of hollow polymer particles and microcapsules by radical polymerization using emulsions consisting of styrene, perfluoro-n-octane, and aqueous SDS (sodium dodecylsulfate) solution is presented.

中空のポリスチレン粒子と炭化水素とフッ素オイルから成るヤヌス液滴のラジカル重合によるマイクロ カプセルの調製

In this article, we have demonstrated a method for producing hollow particles and microcapsules using oil droplets consisting of hydrocarbon oil (styrene) ...