1 التجميعي من N، N &#39;- (ألكان-1، ن diyl) diisonicotinamide <ol style=";text-align:right;direction:rtl"><li style=";text-align:right;direction:rtl"> تجف رقبة واحدة أو ثلاث رقبات الجولة أسفل القارورة في الفرن (100 درجة مئوية، 1 ساعة) لضمان إزالة كل الرطوبة. </li><li style=";text-align:right;direction:rtl"> إضافة حمض isonicotinic الصلبة، أو المشتقة منه، إلى قارورة جنبا إلى جنب مع شريط التحريك المغناطيسي. إذا كان يجند diaminoalkane (ق) هي مواد صلبة في درجة حرارة الغرفة، ثم يضاف 0.5 الخلد (الشامات إلى عدد من حمض isonicotinic) إلى القارورة في هذه المرحلة. </li><li style=";text-align:right;direction:rtl"> سقف الرقبة (ق) من القارورة مع حواجز مطاطية واستبدال الهواء في قارورة مع النيتروجين إما من خلال تيار النيتروجين المستمر أو من خلال استخدام النيتروجين مليئة البالونات. </li><li style=";text-align:right;direction:rtl"> استخدام إبرة الحقن والمحاقن لإضافة ثنائي ميثيل اللامائية أو dimethylsulfoxide (4 مل لكل 500 ملغ من حمض isonicotinic أو حمض 2 ميثيل isonicotinic) لإذابة المادة الصلبة. إذا كانت المواد الصلبة لا تذوب بسهولة، ثم تسخن بلطف الحل. </li><li style=";text-align:right;direction:rtl"> إضافة 7 حكمه الخلد (إلى لجبل حمض isonicotinic المستخدمة) من الترايثلامين (قاعدة ضعيفة) و 0.5 في حكمه الخلد من diaminoalkane. إذا الحل هو السائل في درجة حرارة الغرفة، ثم يضاف 1.5 حكمه الخلد. </li><li style=";text-align:right;direction:rtl"> إضافة واحد يعادل الخلد أنهيدريد 1-propylphosphonic (وكيل اقتران) مع التحريك المستمر والسماح للرد فعل لإكمال أكثر من 5-12 ساعة. </li></ol> 2. تنقية يغاندس <ol style=";text-align:right;direction:rtl"><li style=";text-align:right;direction:rtl"> لbispyridine بروابط إجراؤها باستخدام بروابط diaminoalkane مع 10 أو أكثر من مجموعات الميثيلين، انتظر المنتجات ليعجل من حل كما تقدم التفاعل. </li><li style=";text-align:right;direction:rtl"> لbispyridine بروابط إجراؤها باستخدام diaminooctane، يعجل المنتج عن طريق إضافة ~ 40 مل من الماء. </li><li style=";text-align:right;direction:rtl"> لbispyridine إجراؤها باستخدام diaminoalkanes من سنتين إلى ست مجموعات الميثيلين، إضافة ~ 40 مل من الماء ويسمح للمركبات لبلورة أكثر من 1-3 أيام. </li><li style=";text-align:right;direction:rtl"> جمع كل يجند bispyridine عن طريق الترشيح فراغ وأعد بلورة من حوالي 400-500 مل من الماء المغلي في 200ملغ من يجند. ملاحظة: هناك حاجة إلى مزيد المياه لفترة أطول بروابط bispyridine واجب إلى هم أقل بكثير للذوبان في الماء. </li><li style=";text-align:right;direction:rtl"> إضافة هيدروكسيد الصوديوم KOH و(الرقم الهيدروجيني 9) إلى حل لضمان أن المركبات هي قواعد مجانا عند التبلور. </li></ol> 3. تحضير وتنقية من Dinuclear البلاتين مجمعات <ol style=";text-align:right;direction:rtl"><li style=";text-align:right;direction:rtl"> تذوب بالكامل عبر diamminodichloridoplatinum (II)، transplatin، في الحارة (70-80 درجة مئوية) الماء (150 مل لكل 200 ملغ من transplatin) لإنتاج الحل واضح الملونة الصفراء بقوة. </li><li style=";text-align:right;direction:rtl"> إضافة 0.5 مول من أي ما يعادل يجند bispyridine ويقلب الحل في درجة حرارة حتى يذوب يجند (حل واضح). انتظر الحل لتحويل بالقرب عديم اللون، إيقاف الحرارة، ويقلب في درجة حرارة الغرفة لبضع ساعات إضافية. </li><li style=";text-align:right;direction:rtl"> إزالة المذيب عن طريق التبخر الدوارة، والتي سوف تسفر عن مسحوق أصفر اللون. </li><li style=";text-align:right;direction:rtl"> تنقية، مجمع البلاتين (عناوين) عن طريق إذابة في الحد الأدنى من الماء الدافئ (50 ~ و# 186؛ C). إذا المتبقية المواد الصلبة الملونة الصفراء أو البيضاء موجودة، ثم تصفية هذه قبالة. </li><li style=";text-align:right;direction:rtl"> إضافة الأسيتون إلى حل حتى يتم تشكيل راسب أبيض الذي يبدو أنه شكل البوليمرية من المجمعات المعدنية ويمثل ما يصل إلى 10٪ من الناتج التفاعل. تستمر إضافة الأسيتون (~ إضافية 20-30 مل) حتى يظهر ما لا يزيد راسب. ملاحظة: هذا الراسب الأبيض هو النجاسة. </li><li style=";text-align:right;direction:rtl"> إزالة هذا يعجل من خلال تصفية محتويات من خلال ورق الترشيح النايلون (0.2 ميكرومتر حجم المسام) ودوار تبخر الحل المتبقية للجفاف، والتي سوف تسفر عن المنتج نقية. ملاحظة: إذا لزم الأمر، يمكن إجراء خطوات إضافية ثم الأسيتون هطول حتى مجمع نقية. </li></ol>

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والكتاب ليس لديهم ما يكشف.

في هذا العمل تم توليفها المجمعات dinuclear البلاتين كعوامل مضادة للسرطان المحتملة. في القيام بذلك تم توليفها بروابط سد bispyridine عبر اقتران رد فعل أميد باستخدام حمض isonicotinic وdiaminoalkanes طول متغير. سابقا تم الإبلاغ توليف bispyridine بروابط ونظائرها الميثيل مع 2-8 مجموعات الميثيلين والم...

الأدوية المضادة للسرطان لا تزال واحدة من البلاتين الأسرة الأكثر استخداما من وكلاء في علاج سرطان الإنسان 1. على الرغم من نجاحها، فإنها تقتصر في تطبيقها من خلال الحد من الآثار الجانبية الحادة جرعة 2-4. جرعات محدودة التي يمكن أن تدار على المرضى يعني أيضا أن الأورام يمكن أن تتطور المقاومة 5. كما تستمر هذه، عقاقير جديدة ليتم وضعها لتحسين صورة الآثار الجانبية والتغلب على المقاومة المكتسبة، مثل phenanthriplatin 6 و 7 phosphaplatin. في أواخر 1990s، وضعت المخدرات trinuclear البلاتين، BBR3464 (مخطط 1) 8، وهذا هو ما يصل إلى 1،000 خ أكثر السامة للخلايا في المختبر من أبرز البلاتين المخدرات، سيسبلاتين. BBR3464 هي أيضا قادرة على التغلب على المقاومة التي اكتسبها في لوحة من خطوط الخلايا السرطانية البشرية 9. للأسف، يتم مطابقة النشاط المتزايد للBBR3464 بنسبة 50 - 100 - أضعاف سمية، التييحد استخدامه 10-12. أيضا يتحلل بسهولة في الجسم، وهذا يعني القليل من المخدرات يصل نوى السرطان سليمة 9. Picoplatin هو الدواء البلاتيني وحيدات النوى التي تحتوي على يجند 2 ميثيل البيريدين (مخطط 1) 13. مجموعة الميثيل من هذا الدواء يحميها من هجوم من قبل nucleophiles البيولوجية؛ على وجه الخصوص تحتوي على السيستين والميثيونين الببتيدات / البروتينات 14-16. على هذا النحو، والمخدرات غير مستقر تماما ويحتوي على نسبة أعلى من ذلك بكثير أن يصل نوى السرطان مقارنة مع كل من BBR3464 وسيسبلاتين 17. يعني في خفض تفاعل أيضا picoplatin ديه القصوى التي يمكن تحملها جرعة أعلى بالمقارنة مع BBR3464 وسيسبلاتين 10،18،19. لذا سعى هذا المشروع إلى الجمع بين خصائص BBR3464 وpicoplatin لإنتاج عقاقير جديدة قادرة على التغلب على المقاومة المكتسبة التي تعرض تحسين الاستقرار البيولوجية وأقل حدة جانبية EFFEسنت (على سبيل المثال، الشكل 1). في القيام بذلك، تم إعداد مجموعة من المجمعات البلاتين dinuclear مع bispyridine سد بروابط 20. يتم إجراء بروابط باستخدام ردود الفعل أميد اقتران مع حمض isonicotinic، أو مشتقاته مثل 2-ميثيل حمض isonicotinic، diaminoalkanes طول متغير. رد فعل واحد يعادل الخلد للبروابط مع اثنين من مكافئات مول من transplatin تعطي المجمعات البلاتين المطلوب (مخطط 1).

<table border="0" cellpadding="0" cellspacing="0" width="782">
	<tbody>
		<tr height="24">
			<td height="24" style="height:24px;width:297px;">D2O</td>
			<td style="width:175px;">Aldrich</td>
			<td align="right" style="width:159px;">151882</td>
			<td style="width:152px;">99.9% D</td>
		</tr>
		<tr height="24">
			<td height="24" style="height:24px;width:297px;">DMSO-d6</td>
			<td style="width:175px;">Aldrich</td>
			<td align="right" style="width:159px;">156914</td>
			<td style="width:152px;">99.96% D</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:297px;">1,8-diaminooctane</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">D22401</td>
			<td align="right" style="width:152px;">98%</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:297px;">1,10-diaminodecane</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">D14204</td>
			<td align="right" style="width:152px;">98%</td>
		</tr>
		<tr height="80">
			<td height="80" style="height:80px;width:297px;">1,12-diaminododecane</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">D1,640-1</td>
			<td align="right" style="width:152px;">98%</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:297px;">Isonicotinic acid</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">I17508</td>
			<td align="right" style="width:152px;">99%</td>
		</tr>
		<tr height="120">
			<td height="120" style="height:120px;width:297px;">1-Propylphosphonic anhydride solution</td>
			<td style="width:175px;">Aldrich</td>
			<td align="right" style="width:159px;">431303</td>
			<td style="width:152px;">50 wt% in ethyl acetate</td>
		</tr>
		<tr height="100">
			<td height="100" style="height:100px;width:297px;">Trans-diaminodichloridoplatinum(II)</td>
			<td style="width:175px;">Aldrich</td>
			<td style="width:159px;">P1525</td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Dimethylsulfoxide</td>
			<td style="width:175px;">Sigma-Aldrich</td>
			<td style="width:159px;">Z76855</td>
			<td style="width:152px;">&#62;99.9%, anhydrous</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">N,N&#8217;-dimethylformamide</td>
			<td style="width:175px;">Sigma-Aldrich</td>
			<td align="right" style="width:159px;">227056</td>
			<td style="width:152px;">99.8%, anhydrous</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Triethylamine</td>
			<td style="width:175px;">Sigma-Aldrich</td>
			<td style="width:159px;">T0886</td>
			<td style="width:152px;">&#62;99%</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Nylon filter membranes</td>
			<td style="width:175px;">Whatman</td>
			<td style="width:159px;">7402-004</td>
			<td style="width:152px;">Pore size, 0.2 &#181;m</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Equipment</td>
			<td style="width:175px;"></td>
			<td style="width:159px;"></td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Magnetic stirring hotplate</td>
			<td style="width:175px;"></td>
			<td style="width:159px;"></td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Magnetic stirring bar&#160;</td>
			<td style="width:175px;"></td>
			<td style="width:159px;"></td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Round bottom or three neck flask</td>
			<td style="width:175px;"></td>
			<td style="width:159px;"></td>
			<td style="width:152px;"></td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:297px;">Rubber septums of sufficient size for chosen round bottom or three neck flask</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">5 mL hypodermic syringes</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Hypodermic needles</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Rubber party ballons</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Rubber bands</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="24">
			<td height="24" style="height:24px;width:297px;">A source of N2 gas</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Rotary evaporator</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Drying oven</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">NMR tubes</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">NMR spectrometer</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">500 mL beakers</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:297px;">Glass or plastic pipettes</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

amide coupling reaction for the synthesis of bispyridine-based ligands and their complexation to platinum as dinuclear anticancer agents

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. Isonicotinic acid, or its derivatives, are coupled to variable length diaminoalkane chains under an inert atmosphere in anhydrous DMF or DMSO with the use of a weak base, triethylamine, and a coupling agent, 1-propylphosphonic anhydride. The products precipitate from solution upon formation or can be precipitated by the addition of water. If desired, the ligands can be further purified by recrystallization from hot water. Dinuclear platinum complex synthesis using the bispyridine ligands is done in hot water using transplatin. The most informative of the chemical characterization techniques to determine the structure and gross purity of both the bispyridine ligands and the final platinum complexes is 1H NMR with particular analysis of the aromatic region of the spectra (7-9 ppm). The platinum complexes have potential application as anticancer agents and the synthesis method can be modified to produce trinuclear and other multinuclear complexes with different hydrogen bonding functionality in the bridging ligand.

وتتميز بروابط bispyridine والمجمعات البلاتين dinuclear كل منها بنسبة 1 H، C 13 و 195 قروش NMR (الجدولان 1 و 2)، والتأين electrospray التحليل الطيفي الشامل. نقطة انصهار دقيق يمكن تحديده باستخدام المسح التفاضلي قياس الكالوري والنقاء وأفضل يحددها التحليل ا...

Watch this Scientific Journal Video about Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents at JoVE.com

Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents

يصف هذا البروتوكول استخدام ردود الفعل أميد حمض اقتران isonicotinic وdiaminoalkanes لتشكيل سد بروابط مناسبة للاستخدام في تركيب المجمعات البلاتين متعدد النوى، والتي تجمع بين جوانب من الأدوية المضادة للسرطان وBBR3464 picoplatin.

أميد اقتران رد فعل لتخليق يغاندس مقرها Bispyridine وComplexation لالبلاتين وكلاء المضادة للسرطان Dinuclear

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. ...

amide-coupling-reaction-for-synthesis-bispyridine-based-ligands-their

Research

JoVE Journal

Chemistry

13.8K Views.  The University of Sydney.  يصف هذا البروتوكول استخدام ردود الفعل أميد حمض اقتران isonicotinic وdiaminoalkanes لتشكيل سد بروابط مناسبة للاستخدام في تركيب المجمعات البلاتين متعدد النوى، والتي تجمع بين جوانب من الأدوية المضادة للسرطان وBBR3464 picoplatin. 

Video: Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents

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.

المضادة للسرطان المعادن مجمعات: التجميعي والتقييم السمسة قبل الفحص الإنتقالي العسكري

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

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.

التجميعي تقسيم وبركة وتوصيف الببتيد المكتبة أميد العالي

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

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

A protocol for the synthesis and processing of polycrystalline SrTiO3 ceramics doped non-uniformly with Pr is presented along with the investigation of their thermoelectric properties.

توليف غير موحد العلاقات العامة مخدر SrTiO<sub&gt; 3</sub&gt; سيراميك وخصائص الحرارية منها

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma ...

Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

This paper describes the synthesis and peroxide-modification of nanosize monosodium titanate (nMST), along with an ion-exchange reaction to load the material with Au(III) ions. The synthesis method was derived from a sol-gel process used to produce micron-sized monosodium titanate (MST), with several key modifications, including altering reagent concentrations, omitting a particle seed step, and introducing a non-ionic surfactant to facilitate control of particle formation and growth. The resultant nMST material exhibits spherical-shaped particle morphology with a monodisperse distribution of particle diameters in the range from 100 to 150&#160;nm. The nMST material was found to have a Brunauer-Emmett-Teller (BET) surface area of 285 m2g-1, which is more than an order of magnitude higher than the micron-sized MST. The isoelectric point of the nMST measured 3.34 pH units, which is a pH unit lower than that measured for the micron-size MST. The nMST material was found to serve as an effective ion exchanger under weakly acidic conditions for the preparation of an Au(III)-exchange nanotitanate. In addition, the formation of the corresponding peroxotitanate was demonstrated by reaction of the nMST with hydrogen peroxide.

The surfactant mediated sol-gel synthesis of nanosized monosodium titanate is described, along with preparation of the corresponding peroxide modified material. An ion-exchange reaction with Au(III) is also presented.

التوليف وتفاعل كيمياء Nanosize أحادية الصوديوم ملح التيتان

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

HKUST-1 as a Heterogeneous Catalyst for the Synthesis of Vanillin

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately 200 different odorant compounds in addition to vanillin. The natural extraction of vanillin (from the orchid Vanilla planifolia, Vanilla tahitiensis and Vanilla pompon) represents only 1% of the worldwide production and since this process is expensive and very long, the rest of the production of vanillin is synthesized. Many biotechnological approaches can be used for the synthesis of vanillin from lignin, phenolic stilbenes, isoeugenol, eugenol, guaicol, etc., with the disadvantage of harming the environment since these processes use strong oxidizing agents and toxic solvents. Thus, eco-friendly alternatives on the production of vanillin are very desirable and thus, under current investigation. Porous coordination polymers (PCPs) are a new class of highly crystalline materials that recently have been used for catalysis. HKUST-1 (Cu3(BTC)2(H2O)3, BTC = 1,3,5-benzene-tricarboxylate) is a very well known PCP which has been extensively studied as a heterogeneous catalyst. Here, we report a synthetic strategy for the production of vanillin by the oxidation of trans-ferulic acid using HKUST-1 as a catalyst.

The conversion of trans-ferulic acid to vanillin was achieved by heterogeneous catalysis. HKUST-1 was employed in this synthesis and the essential step in the catalytic process was the generation of unsaturated metal sites. Thus, when the catalyst was activated under vacuum, full vanillin conversion (yield of 95%) was obtained.

HKUST-1 بمثابة محفز غير المتجانسة للتوليف ونيلين

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the development of antibody drug conjugates (ADCs) and nanomedicine, fluorescent microscopy and systems chemistry. For many of these applications, specificity of the bioconjugation method used is of prime concern. The Michael addition of maleimides with cysteine(s) on the target proteins is highly selective and proceeds rapidly under mild conditions, making it one of the most popular methods for protein bioconjugation.
We demonstrate here the modification of the only surface-accessible cysteine residue on yeast cytochrome c with a ruthenium(II) bisterpyridine maleimide. The protein bioconjugation is verified by gel electrophoresis and purified by aqueous-based fast protein liquid chromatography in 27% yield of isolated protein material. Structural characterization with MALDI-TOF MS and UV-Vis is then used to verify that the bioconjugation is successful. The protocol shown here is easily applicable to other cysteine - maleimide coupling of proteins to other proteins, dyes, drugs or polymers.

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

This protocol details the important steps required for the bioconjugation of a cysteine containing protein to a maleimide, including reagent purification, reaction conditions, bioconjugate purification and bioconjugate characterization.

تخليق البروتين Bioconjugates<em&gt; عبر</em&gt; سيستين-maleimide الكيمياء

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

Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single molecule level. An electrostatic self-assembly and covalent fixation (ESA-CF) process is used for the synthesis of the cyclic poly(tetrahydrofuran) (poly(THF)). The diffusive motion of individual cyclic polymer chains in a melt state is visualized using single molecule fluorescence imaging by incorporating a fluorophore unit in the cyclic chains. The diffusive motion of the chains is quantitatively characterized by means of a combination of mean-squared displacement (MSD) analysis and a cumulative distribution function (CDF) analysis. The cyclic polymer exhibits multiple-mode diffusion which is distinct from its linear counterpart. The results demonstrate that the diffusional heterogeneity of polymers that is often hidden behind ensemble averaging can be revealed by the efficient synthesis of the cyclic polymers using the ESA-CF process and the quantitative analysis of the diffusive motion at the single molecule level using the MSD and CDF analyses.

A protocol for the synthesis and characterization of diffusive motion of cyclic polymers at the single molecule level is presented.

توليف دوري البوليمرات وتوصيف تلك الحركة ناشر في الدولة تذوب في واحدة جزيء مستوى

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single ...

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.

إعداد و<em&gt; في المختبر</em&gt; توصيف وكلاء التباين القائم Dendrimer للتصوير بالرنين المغناطيسي

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

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

تركيب أسلاك البلاتين والنيكل والأمثل للأكسجين الحد من الأداء

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Preparation of Stable Bicyclic Aziridinium Ions and Their Ring-Opening for the Synthesis of Azaheterocycles

Bicyclic aziridinium ions were generated by the removal of an appropriate leaving group through internal nucleophilic attack by nitrogen atom in the aziridine ring. The utility of bicyclic aziridinium ions, specifically 1-azoniabicyclo[3.1.0]hexane and 1-azoniabicyclo[4.1.0]heptane tosylate highlighted in the aziridine ring openings by the nucleophile with the release of the ring strain to yield the corresponding ring-expanded azaheterocycles such as pyrrolidine, piperidine and azepane with diverse substituents on the ring in regio- and stereospecific manner. Herein, we report a simple and convenient method for the preparation of the stable 1-azabicyclo[4.1.0]heptane tosylate followed by selective ring opening via a nucleophilic attack either at the bridge or at the bridgehead carbon to yield piperidine and azepane rings, respectively. This synthetic strategy allowed us to prepare biologically active natural products containing piperidine and azepane motif including sedamine, allosedamine, fagomine and balanol in highly efficient manner.

Bicyclic aziridinium ions such as 1-azoniabicyclo[4.1.0]heptane tosylate were generated from 2-[4-tolenesulfonyloxybutyl]aziridine, which was utilized for the preparation of substituted piperidines and azepanes via regio- and stereospecific ring-expansion with various nucleophiles. This highly efficient protocol allowed us to prepare diverse azaheterocycles including natural products such as fagomine, febrifugine analogue and balanol.

إعداد أيونات أزيريدينيوم تربين مستقرة وعلى فتح الحلقة لتوليف أزاهيتيروسيكليس

Bicyclic aziridinium ions were generated by the removal of an appropriate leaving group through internal nucleophilic attack by nitrogen atom in the ...