ص Vicerrectoría لبحوث الدراسات دي بوسجرادو من بواب، وإفشاء للعلم، والمشاريع رقم حظي بتأييد العمل الحالي روي NAT14، 15، 16--زاي-هيس-NAT17. الملابس الجاهزة وذلك بفضل مبرزين (المكسيك) للمنح الدراسية 417887.

1-رد الفعل
<ol><li>وضع في غطاء دخان قارورة فتح جولة 100 مل مع 0.5 mol (29.8 مل) حمض الخليك الجليدية وإضافة 0.051 mol (5.82 مل) من 3، 5-ديميثيلبيريديني و 5 مل ح2س2 (35 في المائة). الاحتفاظ برد الخليط تحت التحريك المغناطيسي المستمر، في درجة حرارة داخلية 80 درجة مئوية ح 5.</li>
	<li>بعد وقت رد الفعل، بارد قارورة إلى 24 درجة مئوية مع الجليد (دو لا فضح حمض الخليك الغازات للجليد)، وقم بتوصيله إلى وحدة تقطير فراغ عالية عن 90-120 دقيقة لإزالة الزائدة من حمض الخليك. تحذير: لا تستخدم المواد الساخنة. الانتظار حتى الأواني الزجاجية تصل إلى درجة حرارة يمكن التحكم فيها. وهذا أيضا تجنب الأبخرة دخول الجزء العلوي من وحدة التقطير.</li>
	<li>إضافة المقطر المياه (10 مل) مرتين لضمان إزالة أي أثر لحمض الخليك وتركيز الخليط كثيرا قدر الإمكان.</li>
</ol>2-باسيسيتي التكيف واستخراج
<ol><li>تذوب في الماء ثنائية ديستيلاتيد المنتج لزج وشفاف معزولة واستخدام الجهد لضبط درجة الحموضة إلى 10 مع نقية الصلبة Na2CO3.</li>
	<li>بعناية بوضع الحل في قمع فصل 250 مل واستخراج 5 مرات مع 250 مل من شكل3 إلى زيادة الغلة. استعادة الطبقة العضوية والجافة على نا الصلبة2حتى4 لمدة 30 دقيقة كحد أقصى، والتي سوف تحتوي على المنتج. إذا لزم الأمر، إعادة استخراج المرحلة المائية مع المبلغ المطلوب من شكل3. تنبيه: تشكل3 قد تسبب النعاس والدوار؛ التعامل مع الرعاية وداخل غطاء دخان.</li>
	<li>إزالة المذيب تحت ضغط انخفاض مع وحدة تقطير فراغ عالية، حتى تشكيل مسحوق بلوري بيج واضحة جداً بلوري (70 في المائة).</li>
</ol>3-بلورة عملية
<ol><li>حل 4.3 غم مسحوق بلوري في 50 مل أثير ثنائي إثيل الصف الباردة عالية اللوني السائل المؤداة ([هبلك]). تصفية الحل لإزالة أي أثر لمواد انطلاق صلبة أو حتى الغبار من فراغ. صب فيلتراتي في كوب طبق بيتري، وتركها لبطء تتبخر في 4 درجات مئوية في ثلاجة مختبر.</li>
	<li>ضمان أن يتم الحصول على بلورات واضحة عديم اللون بعد يومين. ثم قياس نقطة الانصهار، التي ينبغي أن تكون في النطاق من 310-311 ك.</li>
</ol>4-تحليل 3.5-لوتيديني ن-أكسيد ديهيدراتي
<ol><li>إزالة البلورات التي تشكلت، المنشورية الشكل وعديم اللون، قبل والصفق من الجدران قارورة لمزيد من التحليل بالأشعة السينية. إذا كان المستخدم ليس على الفور، تبقى البلورات في الاثير ثنائي إثيل لتفادي ترطيب كريستال.</li>
	<li>حل 0.010 ز 3، 5-لوتيديني ن-أكسيد يذوي في 0.4 مل من كدكل3 لإجراء الرنين المغناطيسي النووي ح1 وج13 تحليل لإثبات فعالية هذا الإجراء.</li>
</ol>

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أن تعلن جميع المؤلفين لا تضارب في المصالح.

البروتوكول المعروضة هنا الطريقة تقليدية لربط ذرة أكسجين إلى ذرة النيتروجين من 3، 5-لوتيديني كطريقة الروغان من ركائز. هذا الأسلوب أيضا راسخة تسفر عن بلورات الأشعة السينية المجففة مناسبة (الشكل 5، صور التقطت بواسطة كاميرا سوني سايبر شوت DSC-HX300). وبقدر ما نشعر بالقلق، ووصفت تقارير كثي?...

في الوقت الحاضر، العلماء في جميع أنحاء العالم وقد تم استثمار الموارد في تطوير طرق اصطناعية جديدة الروغان المجموعات العطرية، التي هي معروفة لجبهة مفاعليه منخفضة بالإضافة إلى ردود فعل1،2، 3. بيريدين، حيث يستبدل ذرة نيتروجين من ذرة الكربون، ويعرض مفاعليه كيميائية مشابهة التناظرية عصابات تتألف من ذرات الكربون3فقط، وأنها عادة ما يخضع إليه الاستعاضة بدلاً من إضافة. ن-أكاسيد مميزة بوجود سند المانحين بين النيتروجين والأكسجين يتكون من التداخل بين زوج إلكترون نونبوندينج على النيتروجين مع المداري فارغة على ذرة الأوكسجين3. وبخاصة، بيريدين ن-أكاسيد قواعد لويس، لأن بها مجموعة N-O قد يعمل كجهة مانحة إلكترون، وأنهم قد ضم مع أحماض لويس تشكيل أزواج حمض-قاعدة لويس المقابلة. هذه الخاصية قد كنتيجة كيميائية أساسية، لأنها زيادة نوكليوفيليسيتي الأحماض لويس نحو اليكتروفيليس المحتملة وهكذا السماح لهم بالرد في ظروف فيها عادة رد فعل لن يحدث. ربما الأكثر شيوعاً استخدام هذه المركبات في مختلف التفاعلات الأكسدة حيث أنها تعمل بمثابة التأكسد4. بيريدين ن-أكاسيد والعديد من مشتقاتها فونكتيوناليزيد خاتم الجزيئات المتكررة من العوامل النشطة بيولوجيا والدوائية5، وقد أنشئت توزيع المكاني واضحة بمختلف الأدوات الطيفية بالنسبة للبعض منهم6،7. في البحوث المتعلقة بربط مختلف المجموعات إلى حلقة بيريدين، اختبرت العلماء منهجيات مختلفة لإنتاج طريقة سهلة وتقليدية، ولما إيسوكسازولينيس يتطلب كمية حفاز من قاعدة مثل الدنمركي في الغليان زيلين نفط إلى الشكل 6- استبدال--2--أمينوبيريديني ن-أكاسيد8،9. مجموعة متنوعة من مشتقات بيريدين تم تحويلها إلى ما يقابلها ن-أكاسيد حضور كمية حفاز من المنغنيز tetrakis(2,6-diclorophenyl) خلات الأمونيوم والبورفيرين في الفصل2Cl2/CH3 أهي8،10. أخرى pyridines تتأكسد أكاسيد استخدام ح2س2 حضور مبالغ الحفاز من ميثيلتريوكسورهينيوم8،11، أو بإضافة ديميثيلديوكسيراني الزائدة في الفصل2Cl2 في 0 درجة مئوية، مما يؤدي إلى أن المقابلة N-أكاسيد8،12،،من1314. مكررا بيروكسيد (تريميثيلسيليل) حضور تريوكسورهينيوم في الفصل2Cl2 قد استخدمت لتوليف بيريدين N-أكاسيد8،11. توليف أمينوبيريديني ن-أكاسيد أسيلاتيون التي تشمل استخدام كارو للحمض (حمض بيروكسومونوسولفوريك) كما تم الإبلاغ عن8. ومع ذلك، المنهجية التي ذكرت هنا، والذي يستخدم جزءا من المنهجية التي أوردها Ochiai1، يقدم نتائج جيدة جداً مع الاستخدام الكواشف أرخص ويمكن الوصول إليها وحاء2يا2 وحمض الخليك الجليدية. هذه الممارسة أكثر مناسبة للاستخدام في الأعمال التحضيرية الواسعة النطاق التي تعمل على الأمينات الثالثية، وتنتج المحاصيل الجيدة في رد فعل لا يتطلب سوى 30% من بيروكسيد الهيدروجين، وحمض الخليك الجليدية في درجة حرارة تتراوح بين 70-80 درجة مئوية، وتستخدم عملية تنقية هذا متاح في معظم المختبرات توليف مثل التقطير، دون استخدام محفز أو أغلى الكواشف1. تقارير الأدب أن المنهجيات الأخرى أيضا في كثير من الأحيان تشمل الأطر الزمنية من 10-24 ح ودرجات حرارة فوق 100 درجة مئوية 4،8، ونادراً ما ذكر عائد البلورات بشكل جيد للتحاليل بالأشعة السينية.
رجعي، ومختلف أكسيد مشتقات N-تستخدم لتنشيط الحلبة لوتيديني، على نحو كاف في كلتا الحالتين تفاعلات أو اليكتروفيليك. يتأثر عامل تفاعلات أو اليكتروفيليك سوبستيتوينتس. مع عصابة بيريدين يجري المجموعات سحب الإلكترون، هو العامل الرئيسي مميزة تفاعلات1. مجاناً ن-مركبات أكسيد معزولة نادراً ما كبلورات مناسبة لتحليل الأشعة السينية بسبب تهمة الطابع في حلقة عطرية. عامل المذيب غير حاسمة بالنسبة لاستقرار كثافة الأكسجين15سلبية.

<table border="0" cellpadding="0" cellspacing="0" style="width:725px;" width="725">
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		<col />
		<col />
		<col />
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	<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>
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syntheses, crystallization, and spectroscopic characterization of 3,5-lutidine n-oxide dehydrate

التوليف من 3، 5-لوتيديني ن-أكسيد يذوي، 1، تحقق في مسار توليف حمض 2-أمينو-بيريدين-3، 5-ديكاربوكسيليك. Ochiai أول من استخدم المنهجية لعدم استبدال بيريدينيس في عام 1957 في عملية ح 12، ولكن تم الحصول على بلورات مناسبة لا الأشعة السينية. وضوح تأثير الحلبة المستبدلة المستخدمة في المنهجية المقدمة هنا إضافة جزيئات الماء في الوحدة غير متماثلة، مما يمنح قوة تفاعلات مختلفة في 1. مجمع الكريستال مناسبة 1 الأشعة السينية كان ممكناً بفضل استقرار شحنة سالبة في الأكسجين بسبب وجود اثنين من جزيئات الماء حيث أن ذرات الهيدروجين التبرع بتهمة إيجابية إلى الحلبة؛ هذه الجزيئات المائية تخدم جيدا لبناء تفاعل سوبراموليكولار. قد يكون من الممكن للنظام القلوي الذي يتم الوصول إليه عن طريق ضبط درجة الحموضة إلى 10 جزيئات رطب. الأهم من ذلك، استبدال الميثيل مزدوجة خاتم ووقت رد الفعل من ح 5، يجعل من أسلوب أكثر تنوعاً ومع التطبيقات الكيميائية الأوسع نطاقا للملاحق خاتم مستقبلا.

البروتوكول أساسا امتداداً ل Ochiai في أسلوب1. ومع ذلك، يتم تطبيق حرارة أقل ووقتاً أقل. يمكن استخدام هذه الطريقة البسيطة للحصول على يجند تنوعاً، وبيريدين المستبدلة ن-أكسيد متفرعة. للتأكد من تكوين 1، يفضل الرنين المغناطيسي 1ح و 13ج التحليل...

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

هنا، نحن تقرير التوليف وتبلور 3.5-لوتيديني ن-أكسيد يذوي بموجب بروتوكول بسيط يختلف عن توليف بيريدين نالكلاسيكية-أكسيد. هذا البروتوكول يستخدم مواد انطلاق مختلفة، وينطوي على أقل وقت رد الفعل تؤتي ومذاوبة سوبراموليكولار هيكل جديد، الذي يبلور تحت التبخر بطيئة.

التوليفات وتبلور، وتوصيف الطيفية من 3، 5-لوتيديني ن-أكسيد يذوي

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

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Chemistry

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

8.3K Views.  Benemérita Universidad Autónoma de Puebla. هنا، نحن تقرير التوليف وتبلور 3.5-لوتيديني ن-أكسيد يذوي بموجب بروتوكول بسيط يختلف عن توليف بيريدين نالكلاسيكية-أكسيد. هذا البروتوكول يستخدم مواد انطلاق مختلفة، وينطوي على أقل وقت رد الفعل تؤتي ومذاوبة سوبراموليكولار هيكل جديد، الذي يبلور تحت التبخر بط...

Video: 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.

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 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.

أطر توليف وتوصيف بين functionalized المعدنية العضوية

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.

نشر الانعكاس الطيفي بالأشعة تحت الحمراء تحديد مشتتة / الجسيمات الربط آليات في الأحبار وظيفية

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.

تعليق السطح القائم على تصفية المحسن رامان الطيفي الفحص للكشف السريع من الملوثات الكيميائية

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.

توليف وتوصيف المواد الغروية Supramolecular

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.

موقع إخراج صفها سبين والثوري دراسات طيفية القنوات Pentameric يجند بوابات ايون

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.

إعداد وتوصيف ج60/Graphene الهجين النانو

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.

توليف لكتلة الإنشاء ثيول لبلورة إطار جيرويدال معدن الكبريت انتشارية

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.

تبلور الغرواني الكهربي الأغشية سامسونج إطار المعادن العضوية عالية الأداء

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.

تركيب وتوصيف جسيمات نانوية الذهب أمفيفيليك

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