Name: a microwave-assisted direct heteroarylation of ketones using transition metal catalysis
Uploaded: 2020-02-16T13:00:00
Description: Watch this Scientific Journal Video about A Microwave-Assisted Direct Heteroarylation of Ketones Using Transition Metal Catalysis at JoVE.com

向美国化学学会石油研究基金的捐赠者表示认可，以支持这项研究（PRF# 54968-UR1）。这项工作也得到了国家科学基金会（CHE-1760393）的支持。我们感谢NKU科学与数学一体化中心、NKU-STEM国际研究计划以及化学和生物化学系在财政和后勤方面的支持。我们还感谢伊利诺伊大学厄巴纳-香槟分校化学科学学院质谱实验室获得HRMS数据。

谨慎：
<ul><li>对于配备 4 x 24MG5 转子的微波反应器，微波反应小瓶应在 20 bar 下运行。如果反应使用非常挥发性的溶剂，产生气体，或者如果溶剂分解，有必要计算压力在某些反应温度下，以确保小瓶的总压力小于20巴。</li>
	<li>本议定书采用手套箱、闪式色谱和核磁共振（NMR）有机合成的标准技术。</li>
	<li>实验期间应使用适当的个人防护设备 （PPE）。其中包括安全护目镜、实验室外套、单体?...

<ol>
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On the Question of the Nonthermal Microwave Effect.</a> The Journal of Organic Chemistry. 68 (23), 9136-9139 (2003).</li><li>Amato, E., 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=Investigation+of+fluorinated+and+bifunctionalized+3-phenylchroman-4-one+(isoflavanone)+aromatase+inhibitors.">Investigation of fluorinated and bifunctionalized 3-phenylchroman-4-one (isoflavanone) aromatase inhibitors.</a> Bioorganic &amp; Medicinal Chemistry. 22 (1), 126-134 (2014).</li><li>Bonfield, K., 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=Development+of+a+new+class+of+aromatase+inhibitors:+Design,+synthesis+and+inhibitory+activity+of+3-phenylchroman-4-one+(isoflavanone)+derivatives.">Development of a new class of aromatase inhibitors: Design, synthesis and inhibitory activity of 3-phenylchroman-4-one (isoflavanone) derivatives.</a> Bioorganic &amp; Medicinal Chemistry. 20 (8), 2603-2613 (2012).</li><li>Y&#305;lmaz, F., Mentese, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Rapid+Protocol+for+the+Synthesis+of+N-[2-(alkyl/aryl)-4-phenyl-1Himidazol-1-yl]+benzamides+via+Microwave+Technique.">A Rapid Protocol for the Synthesis of N-[2-(alkyl/aryl)-4-phenyl-1Himidazol-1-yl] benzamides via Microwave Technique.</a> Current Microwave Chemistry. 1 (1), 47-51 (2014).</li><li>Xia, Y., Chen, L. Y., Lv, S., Sun, Z., Wang, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microwave-Assisted+or+Cu-NHC-Catalyzed+Cycloaddition+of+Azido-Disubstituted+Alkynes:+Bifurcation+of+Reaction+Pathways.">Microwave-Assisted or Cu-NHC-Catalyzed Cycloaddition of Azido-Disubstituted Alkynes: Bifurcation of Reaction Pathways.</a> The Journal of Organic Chemistry. 79 (20), 9818-9825 (2014).</li><li>Lei, C., Jin, X., Zhou, J. 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S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+facile,+microwave-assisted,+palladium-catalyzed+arylation+of+acetone.">A facile, microwave-assisted, palladium-catalyzed arylation of acetone.</a> Tetrahedron Letters. 48 (7), 1213-1216 (2007).</li><li>Amat, M., Hadida, S., Pshenichnyi, G., Bosch, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Palladium(0)-Catalyzed+Heteroarylation+of+2-+and+3-Indolylzinc+Derivatives.+An+Efficient+General+Method+for+the+Preparation+of+(2-Pyridyl)indoles+and+Their+Application+to+Indole+Alkaloid+Synthesis.">Palladium(0)-Catalyzed Heteroarylation of 2- and 3-Indolylzinc Derivatives. An Efficient General Method for the Preparation of (2-Pyridyl)indoles and Their Application to Indole Alkaloid Synthesis.</a> The Journal of Organic Chemistry. 62 (10), 3158-3175 (1997).</li><li>Tennant, G. J., Wallis, C. W., Weaver C, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+the+first+examples+of+the+imidazo[4,5-c]isoxazole+ring+system.">Synthesis of the first examples of the imidazo[4,5-c]isoxazole ring system.</a> Journal of the Chemical Society, Perkin Transactions. 1, 817-826 (1999).</li><li>Spergel, S. H., Okoro, D. R., Pitts, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=One-Pot+Synthesis+of+Azaindoles+via+Palladium-Catalyzed+&#945;-Heteroarylation+of+Ketone+Enolates.">One-Pot Synthesis of Azaindoles via Palladium-Catalyzed &#945;-Heteroarylation of Ketone Enolates.</a> The Journal of Organic Chemistry. 75 (15), 5316-5319 (2010).</li><li>Jiang, Y., Liang, G., Zhang, C., Loh, T. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Palladium-Catalyzed+C-S+Bond+Formation+of+Stable+Enamines+with+Arene/Alkanethiols:+Highly+Regioselective+Synthesis+of+&#946;-Amino+Sulfides.">Palladium-Catalyzed C-S Bond Formation of Stable Enamines with Arene/Alkanethiols: Highly Regioselective Synthesis of &#946;-Amino Sulfides.</a> European Journal of Organic Chemistry. 2016 (20), 3326-3330 (2016).</li><li>King, S. M., Buchwald, S. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+a+Method+for+the+N-Arylation+of+Amino+Acid+Esters+with+Aryl+Triflates.">Development of a Method for the N-Arylation of Amino Acid Esters with Aryl Triflates.</a> Organic Letters. 18 (16), 4128-4131 (2016).</li><li>Ge, S., Hartwig, J. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nickel-catalyzed+asymmetric+alpha-arylation+and+heteroarylation+of+ketones+with+chloroarenes:+effect+of+halide+on+selectivity,+oxidation+state,+and+room-temperature+reactions.">Nickel-catalyzed asymmetric alpha-arylation and heteroarylation of ketones with chloroarenes: effect of halide on selectivity, oxidation state, and room-temperature reactions.</a> The Journal of the American Chemical Society. 133 (41), 16330-16333 (2011).</li><li>Quillen, A., 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=Palladium-Catalyzed+Direct+&#945;-C(sp3)+Heteroarylation+of+Ketones+under+Microwave+Irradiation.">Palladium-Catalyzed Direct &#945;-C(sp3) Heteroarylation of Ketones under Microwave Irradiation.</a> The Journal of Organic Chemistry. 84 (12), 7652-7663 (2019).</li><li>Kremsner, J. M., Kappe, C. O. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Silicon+Carbide+Passive+Heating+Elements+in+Microwave-Assisted+Organic+Synthesis+-+SI.">Silicon Carbide Passive Heating Elements in Microwave-Assisted Organic Synthesis - SI.</a> The Journal of Organic Chemistry. 71 (12), 4651-4658 (2006).</li><li>Erythropel, H. C., 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=The+Green+ChemisTREE:+20+years+after+taking+root+with+the+12+principles.">The Green ChemisTREE: 20 years after taking root with the 12 principles.</a> Green Chemistry. 20 (9), 1929-1961 (2018).</li><li>Barge, A., Tagliapietra, S., Tei, L., Cintas, P., Cravotto, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pd-catalyzed+reactions+promoted+by+ultrasound+and/or+microwave+irradiation.">Pd-catalyzed reactions promoted by ultrasound and/or microwave irradiation.</a> Current Organic Chemistry. 12 (18), 1588-1612 (2008).</li><li>Kimura, M., Mukai, R., Tanigawa, N., Tanaka, S., Tamaru, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Triethylborane+as+an+efficient+promoter+for+palladium-catalyzed+allylation+of+active+methylene+compounds+with+allyl+alcohols.">Triethylborane as an efficient promoter for palladium-catalyzed allylation of active methylene compounds with allyl alcohols.</a> Tetrahedron. 59 (39), 7767-7777 (2003).</li></ol>

本文描述的方法是为了获取有价值的合成基块 - 异丙基化合物。与异质化的先例文献报告相比，目前这种催化系统的选择显示出几个显著的优势。首先，它避免了保护组的使用、反应中间体的分离、催化剂的化学测量要求以及延长反应时间11、17。其次，SiC板为以多样性为导向的药物发现提供并行合成的大好机会19。理论上，在微波照?...

微波通过离子传导或双极极极化与材料相互作用，提供快速均匀的加热。微波辅助有机反应自1986年首次报告快速有机合成报告后，在研究实验室中越来越受欢迎。虽然微波加热的确切性质尚不明确，而且"非热"微波效应的存在仍在争论之中，但已观察到微波辅助有机反应的显著速率增强，并报道了2。据报道，在微波照射下，通常需要数小时或数天才能完成的缓慢反应，在几分钟内完成。据报告，在微波照射下，需要高活化能量（如循环和进行固菌阻碍的场址结构）的困难有机反应是成功的，反应产量和纯度提高7。微波辅助有机合成结合无溶剂反应和多米诺骨牌反应等其他特性，在环保反应设计方面具有无可比拟的优势。
与被广泛研究的基质等价物不同，异质化，特别是在碳基化合物的β-C（sp3）上，在文献中很少报道。少数关于碳基化合物α-异质化的文献报告具有很大的局限性，如催化剂的化学计量量、狭窄的基质范围和反应中间体的分离11、12、13。酮子的直接异质化仍有待解决，以便使其成为一种通用方法。首先，异原子倾向于协调过渡金属催化剂，导致催化剂中毒14，15。其次，单体（异质）消融产物中的β-H比起始材料中的β-H更酸性。因此，它倾向于进一步反应，使不需要的（双食）内化或（多角质）内化产物。第三，碳基化合物的成本通常低于二甲基化合物，因此使用多余的碳基化合物来推动反应完成是切实可行的。然而，过量的碳基化合物往往会导致自冷凝，这是碳基化合物过渡金属催化+异化中经常遇到的一个问题。
在这份报告中，我们描述了我们最近对使用微波辅助反应方案直接β-C（sp3）酮异化的研究。为了应对第一个挑战，上面讨论的催化剂中毒，使用强协调和消毒阻碍配体，以尽量减少异原子的催化剂中毒。大块的配体也有望减缓侧反应，如（双流）内化或（多角质）16，17，上述第二个挑战。为了尽量减少第三个挑战的影响，形成酮自冷凝侧产品，采用了2个以上等价的碱基，将酮转化为相应的依有物。反应时间长、反应温度高，加上酮子直接β-C（sp3）异质化的挑战，使其成为微波辅助有机合成研究的合适人选。

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>Chloroform-d (99.8+% atome D)</td>
			<td>Acros Organics</td>
			<td>AC209561000</td>
			<td>contains 0.03 v/v% TMS</td>
		</tr>
		<tr>
			<td>CombiFlash Rf Flash Chromatography system</td>
			<td>Teledyne Isco</td>
			<td></td>
			<td>automated flash chromatography system</td>
		</tr>
		<tr>
			<td>CombiFlash Solid load catridges (5 gram)</td>
			<td>Teledyne Isco</td>
			<td>69-3873-235</td>
			<td>disposable</td>
		</tr>
		<tr>
			<td>CombiFlash prepacked column (4g)</td>
			<td>Teledyne Isco</td>
			<td>69-2203-304</td>
			<td>RediSep Rf silica 40-60 um, disposable</td>
		</tr>
		<tr>
			<td>Microwave Reactor - Multiwave Pro</td>
			<td>Anton Paar</td>
			<td>108041</td>
			<td>Microwave Reactor</td>
		</tr>
		<tr>
			<td>Microwave Reactor Rotor 4X24 MG5</td>
			<td>Anton Paar</td>
			<td>79114</td>
			<td>for parallel organic synthesis with with 4 SiC Well Plate 24</td>
		</tr>
		<tr>
			<td>Microwave reaction vials</td>
			<td>Wheaton&#174; glass</td>
			<td>224882</td>
			<td>disposible, 13-425, 15x46 mm, reaction solution 0.3 - 3.0 mL, working pressure 20 bar</td>
		</tr>
		<tr>
			<td>Microwave reaction vial seals, set</td>
			<td>Anton Paar</td>
			<td>41186</td>
			<td>made of Teflon; disposable</td>
		</tr>
		<tr>
			<td>Microwave reaction vial screw cap</td>
			<td>Anton Paar</td>
			<td>41188</td>
			<td>made of PEEK; forever reusable</td>
		</tr>
		<tr>
			<td>Microwave reaction vial stirring bar</td>
			<td>CTechGlass</td>
			<td>S00001-0000</td>
			<td>Magnetic, PTFE, Length 9mm. Diameter: 3mm. (Package of 5)</td>
		</tr>
		<tr>
			<td>NaOtBu</td>
			<td>Sigma-Aldrich</td>
			<td>703788</td>
			<td>stored in a glovebox under nitrogen atmosphere</td>
		</tr>
		<tr>
			<td>Nuclear Magnetic Resonance Spectrometer</td>
			<td>Joel</td>
			<td></td>
			<td>500 MHz spectrometer</td>
		</tr>
		<tr>
			<td>Silica gel</td>
			<td>Teledyne Isco</td>
			<td>605394478</td>
			<td>40-60 microns, 60 angstroms</td>
		</tr>
		<tr>
			<td>Toluene</td>
			<td>Sigma-Aldrich</td>
			<td>244511</td>
			<td>vigorously purged with argon for 2 h before use</td>
		</tr>
		<tr>
			<td>XPhos Palladacycle Gen. 4 Catalyst</td>
			<td>STREM</td>
			<td>46-0327</td>
			<td>stored in a glovebox under nitrogen atmosphere</td>
		</tr>
		<tr>
			<td>various ketones</td>
			<td>Sigma-Aldrich or Fisher or Ark Pharm.</td>
			<td></td>
			<td>substrates for heteroarylation</td>
		</tr>
		<tr>
			<td>various heteroaryl halides</td>
			<td>Sigma-Aldrich or Fisher or Ark Pharm.</td>
			<td></td>
			<td>substrates for heteroarylation</td>
		</tr>
	</tbody>
</table>

a microwave-assisted direct heteroarylation of ketones using transition metal catalysis

异质化将异位基片段引入有机分子。尽管通过过渡金属催化报告有无数关于直接异化的可有反应，但关于直接异质化的文献很少。由于催化剂中毒、产物分解等异质原子的存在，异质化常常使异化成为一个具有挑战性的研究领域，包括催化剂中毒、产物分解等。该协议详细介绍了在微波辐照下酮的高效直接β-C（sp3）异射。成功异质化的关键因素包括使用XPhos PalladacycleGen 4催化剂、过量碱以抑制侧反应以及微波照射下密封反应小瓶中实现的高温和压力。该方法制备的异质化化合物具有质子核磁共振光谱（1H NMR）、碳核磁共振光谱（13CNMR）和高分辨率质谱（HRMS）等特征。该方法与文献先例具有若干优点，包括广泛的基底范围、快速反应时间、更环保的程序和操作简便性，消除了硅醇醚等中间体的制备。该协议的可能应用包括但不限于用于发现生物活性小分子的以多样性为导向的合成、用于制备天然产物的多米诺骨牌合成以及用于新过渡金属催化系统的配体开发。

可采用这种高效的微波辅助协议，对酮的直接β-C（sp3）异质化进行。本研究中合成的杂酮的选定示例如图1所示。具体来说，化合物1a被合成并分离为淡黄色油（0.49毫摩尔，192毫克，98%）。其1H 和13C NMR 光谱如图2所示，用于确认结构和纯度。在 1H 频谱中存在双质子单一信号 ± 4.26 ppm，证实了酮 + 碳和杂基卤化物之?...

Watch this Scientific Journal Video about A Microwave-Assisted Direct Heteroarylation of Ketones Using Transition Metal Catalysis at JoVE.com

A Microwave-Assisted Direct Heteroarylation of Ketones Using Transition Metal Catalysis

杂性化合物是有机合成、药用和生物化学中的重要分子。微波辅助异质化，使用铂催化提供了一种快速而有效的方法，将异丙烯基直接附着在酮基材上。

利用过渡金属催化的酮的微波辅助直接异化

Heteroarylation introduces heteroaryl fragments to organic molecules. Despite the numerous available reactions reported for arylation via transition metal ...

该协议利用微波辐照和铂催化剂直接在酮的α碳上附加异体片段。该技术的主要优点是快速构建异体化合物，用于药用化学筛选、催化剂辅助开发以及串联有机反应发现。我们研究的长期意义是合成一种有效的芳香酶抑制剂，作为激素受体阳性乳腺癌的潜在治疗。使用手套箱时，错误很可能来自溢出，因此我们的建议是花点时间，因为反应不需要快速的步伐才能成功。将所需的试剂和用品运送到手套箱中。在栖息的手套箱内，重达115毫克的三氧化钠直接放入四毫升微波反应小瓶中。使用玻璃移液器将一毫升脱气甲苯加入微波反应小瓶中。重量9毫克的XPhos帕拉达环第4代催化剂，并将其添加到微波小瓶。将铲入小瓶中的溶液中，并旋转，以确保催化剂的完全转移。然后，使用合适的微升注射器将64.4微升的乙酰苯酮加入微波小瓶。重103毫克的3-碘二丁，并添加到微波小瓶。接下来，再加入一毫升脱气甲苯，使总反应混合物约三毫升。仔细将密封件和盖子连接起来，并放在微波反应小瓶上。拧紧。把化学品、用品和垃圾从手套箱里拿出来。将组装的反应小瓶放在微波反应器上，并放在转子上的碳化硅板上。对于多个反应小瓶，将它们均匀地放在转子上的四个碳化硅板上。将红外传感器温度限制设置为 113 摄氏度，与 130 摄氏度的实际反应温度相对应。根据手稿对每一步的微波功率和时间进行编程。在微波照射下运行反应。记录实际反应时间和温度。微波反应小瓶冷却至环境温度后，将反应混合物转移到分离漏斗中，并用少量乙酸乙酯冲洗到漏斗中。将两毫升的饱和氯化铵和十毫升乙酸乙酯加入分离漏斗，然后摇动混合。将分离漏斗放在机架上，以放置五分钟。打开阀门排出水层，然后分离顶部有机层，将其保存在干净、干燥的烧杯中。重复提取，再加入十毫升乙酸乙酸乙酯两次，并结合有机层。干燥和旋转蒸发后，记录粗制质产品的形状、颜色和质量。使用自动闪光色谱验证最终产品。首先，将粗制产品溶解在一到两毫升丙酮中，放在一个圆底烧瓶中，然后加入1.5克硅胶，制作浆料。进行旋转蒸发约五分钟，非常小心地去除丙酮，使产品被装在硅胶上。将生成的硅胶转移到空的闪光色谱加载盒中。为自动 MPLC 系统组装装料盒、预装柱、试管机架和溶剂管。为 MPLC 系统设置溶剂梯度和其他参数并运行闪光色谱。将所需的 MPLC 馏分混合在圆底烧瓶中，并将溶剂蒸发在旋转蒸发装置上，以收集纯产品。在高真空下干燥纯化产品至少一小时，以去除残留溶剂。然后，重达5至10毫克的最终纯化产品。溶解0.75毫升的脱化氯仿或其他适当的脱盐溶剂。并采取质子核磁共振谱。利用这种高效的微波辅助协议，对酮进行了直接α-碳异质化。例如，化合物1A被合成并分离为淡黄色化合物。此处显示了其质子和碳-13 NMR光谱。质子光谱中三角洲4.26 ppm的两质子单体信号的存在证实了酮和异丙烯卤化物之间的成功碳-碳耦合。基于乙酸乙酯和六烷溶剂系统的纯化，使化合物与一个氮的分离效果良好。当该方法用于具有两个或两个或更多氮原子的化合物时，应采用甲醇和二氯甲烷溶剂系统来更快地洗脱。要记住的最重要的事情是确保所有试剂，特别是催化剂的准确和完整转移。该技术允许研究人员进行平行合成，以发现药物试剂，并开发多米诺骨牌方法的自然产品合成。

Research

Education

JoVE Journal

JoVE Core

Chemistry

Cell Biology

Organic Chemistry

Unit 1

Aldehydes and Ketones

Biochemistry of the Cell

SCIENTISTS IN ACTION

Microwave-assisted Intramolecular Dehydrogenative Diels-Alder Reactions for the Synthesis of Functionalized Naphthalenes/Solvatochromic Dyes

微波辅助分子内Diels-Alder反应的功能化萘/变色染料的合成脱氢

Functionalized naphthalenes have applications in a variety of research fields ranging from the synthesis of natural or biologically active molecules to ...

科研

化学

Microwave-assisted Functionalization of Poly(ethylene glycol) and On-resin Peptides for Use in Chain Polymerizations and Hydrogel Formation

Microwave-assisted Functionalization of Polyethylene glycol and On-resin Peptides for Use in Chain Polymerizations and Hydrogel Formation

保利的微波辅助功能化（乙二醇）和On-树脂链聚合反应，并形成水凝胶的肽使用

One of the main benefits to using poly(ethylene glycol) (PEG) macromers in hydrogel formation is synthetic versatility. The ability to draw from a large ...

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

单金属和双金属前过渡金属碳化物和氮化物纳米粒子的反相微乳液介导的合成

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

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

植物材料的快速高通量物种鉴定实时高分辨质谱法直接分析

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

One-pot Microwave-assisted Conversion of Anomeric Nitrate-esters to Trichloroacetimidates

硝酸酯 Anomeric Trichloroacetimidates 的单锅微波辅助转化

The goal of the following procedure is to provide a demonstration of the one-pot conversion of a 2-azido-1-nitrate-ester to a trichloroacetimidate ...

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

电化学 CO2还原的过渡金属单原子催化剂的合成及性能表征

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

Separation of Aldehydes and Reactive Ketones from Mixtures Using a Bisulfite Extraction Protocol

用亚硫酸氢萃取协议分离混合物中的醛和反应性酮

The purification of organic compounds is an essential component of routine synthetic operations. The ability to remove contaminants into an aqueous layer ...

Reducing Willow Wood Fuel Emission by Low Temperature Microwave Assisted Hydrothermal Carbonization

低温微波辅助热液碳化降低柳树燃料排放

Biomass is a sustainable fuel, as its CO2 emissions are reintegrated in biomass growth. However, the inorganic precursors in the biomass cause a negative ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

利用表面有机金属化学方法，利用硅支持的催化剂进行Imine金属分析

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...