The authors acknowledge funding from Fonds de Recherche du Qu&#233;bec - Nature et Technologies, from Conseil Recherches en Sciences Naturelles et G&#233;nie (program INNOV) and PrimaQu&#233;bec.

1.聚（5-降冰片烯-2-羧酸），PNBE制备（CO 2 H） <ol><li> 单体NBE制备（CO 2 H） <ol><li>称出丙烯酸（AA）（327克，4.5摩尔，2当量）和氢醌（4.9克，4.5×10 -2摩尔，0.02当量），并将它们添加到装有冷凝器的2升圆底烧瓶中和磁力搅拌棒。加热使用的硅油浴中在150℃的烧瓶中。 </li><li>一旦回流解决，在一个单一的部分添加的DCPD（300克，2.3摩尔，1当量），然后将温度升至170℃。 </li><li>离开在该温度下16小时的反应。观察由清晰到黄棕色的颜色变化。 </li><li>采取通过用巴斯德吸移管提取一个样本，并通过1 H核磁共振（使用CDCL 3为溶剂）15进行分析。观察NBE的（6.0和6.5 ppm时， 图2顶部之间的双键的信号）的幽灵。 16 </s达&gt; </li></ol></li><li> NBE的纯化（CO 2 H） <ol><li>与连接到在其中冷水循环的冷凝器的简单蒸馏装置（一个平台）替换冷凝器。 </li><li>把反应设置设定为约真空下。 1毫米汞柱。加热在100℃下的混合物中，并收集澄清的液体（ 约 40毫升），其可以被丢弃。 </li><li>更换了500毫升圆底烧瓶中的收集烧瓶。加热油浴至155℃，并观察NBE的滴加蒸馏（CO 2 H）（317克，2.3摩尔产率= 98％）。蒸馏接管7小时。 </li><li>通过1 H NMR分析无色液体，以评估纯度以及具有内切:外切比例（ 图2，底部）。 15 远藤:与用于蒸馏以及与用于粗NBE（CO 2 H）的制备在加热时的时间外型比的变化。通常情况下， 内:外切（在这种情况下，60:40）50:50和80:20，得到之间的比率。 </li></ol></li><li> NBE的聚合（CO 2 H） <ol><li>放置NBE（CO 2 H）300克（2.3摩尔，5000当量）在配备有磁力搅拌棒的500mL圆底烧瓶中。脱气通过鼓泡氮气30分钟的液体。 </li><li>权衡烯丙基钯（Ⅱ）氯化物二聚体，[的PdCl（C 3 H 5）] 2（76毫克，4.2×10 -1毫摩尔，1当量的Pd）并将其添加到该溶液中。添加银锑AgSbF 6（180毫克，5.2×10 -1毫摩尔，1.2当量）。 </li><li>在搅拌下，溶解通过加热钯盐在70℃，并在轻微的氮气通量下维持在70℃的温度。 7至8小时后，搅拌因粘度增加停止。 </li><li>停止36小时后的反应。 </li><li>冷却用液氮的圆底烧瓶中。用抹刀，打破聚合物切成小块。 </li><li>在一个2L烧杯球菌pped有磁性搅拌棒，加入750毫升乙酸乙酯。聚合物块加入到剧烈搅拌下的乙酸乙酯中。继续搅拌2小时。 </li><li>过滤过配备有纸过滤器（413级，直径15厘米）15厘米直径的布氏漏斗将溶液。 </li><li>洗用乙酸乙酯聚合物萃取三次（500毫升，每次洗涤）。干烤箱12小时设定在50℃的真空中的聚合物（123克，9.4×10 -1摩尔，产率= 41％）。 </li></ol></li></ol> 2. PNBE制备（乙烯基） <ol><li> NBE的聚合（乙烯基） <ol><li>脱气甲苯（ 约 200毫升）和NBE（乙烯基）（ 约 200毫升）与N 2鼓泡30分钟，并放置在一个手套箱中。 </li><li>内的手套箱，负载甲苯（100克）的250毫升圆底烧瓶中。 </li><li>中添加Pd 2（DBA）3（76毫克，1.6×10 -1毫摩尔，钯的1当量），AgSbF 6（68毫克，2.0×10 -1米摩尔，1.2当量）和三苯基膦，PPH 3（43毫克，1.6×10 -1毫摩尔，1当量）先后向甲苯溶液。 </li><li>将混合物加热至70℃直至完全溶解发生。它发生在10分钟内。 </li><li> NBE（乙烯基）将100克（8.0×10 -1摩尔，5000当量）添加到该紫色溶液。 </li><li>搅拌在70℃下72小时。 </li><li>除去从手套箱的溶液中，将粘性黑色溶液转移到含磁性搅拌棒的1L玻璃瓶中。 </li><li>添加甲苯（200毫升），并搅拌。 </li><li>添加二氧化硅粉末（硅胶40-63微米，10克）。在室温下搅拌16小时。 </li><li>停止搅拌并让粉末沉降至少2小时，以使二氧化硅粒子到sedimentate。 </li><li>过滤过配备有纸过滤器（413级，直径15厘米）15厘米直径的布氏漏斗将溶液。避免在布氏漏斗浇沉淀二氧化硅颗粒。 </li><li>冲洗二氧化硅相提并论用甲苯（50毫升）ticles并通过布氏漏斗过滤。 </li><li>添加甲醇（1.2L），以装备有磁性搅拌棒的4升烧杯中。 </li><li>添加所有含逐渐下剧烈搅拌聚合物与甲醇的甲苯溶液，并继续搅拌30分钟。 </li><li>过滤过配备有纸过滤器（413级，直径15厘米）15厘米直径的布氏漏斗的聚合物。用甲醇三个等份（400毫升每）洗涤聚合物。改变每次洗涤之间的滤纸。 </li><li>评估通过1 H NMR测定的聚合物的纯度在CDCl 3中，以查看是否残留单体存在（6.0和6.3 ppm的之间的双键信号）。 15，16如果是这样的情况下，继续用甲醇洗涤。 </li><li>干，在室温下真空聚合物（75克，6.3×10 -1摩尔，产率= 78％）中过夜。 </li></ol></li></ol> 3。PNBE的制备（环氧树脂） <ol><li> PNBE的环氧化（乙烯） <ol><li> 150克二氯甲烷添加到配备有磁力搅拌器和冷凝器的500mL圆底烧瓶中。 </li><li>搅拌直至完全溶解添加PNBE（乙烯基）（15克，1.3×10 -1摩尔，1当量）。 </li><li>放置烧瓶在冰浴中，让其冷却15分钟。 </li><li>在一个单独的容器中，混合在一起甲酸（30克，6.5×10 -1摩尔，5当量）和乙酸（5克，8.3×10 -2摩尔，0.6当量）。将合并的酸加入到聚合物溶液中。 </li><li>让它冷却15分钟。 </li><li>添加过氧化氢水溶液（30％）（75克，6.5×10 -1摩尔，5当量）在聚合物溶液中。 </li><li>搅拌18小时。冰浴并不需要被去除，随着温度将逐渐增加至室温。 </li><li>取少量样品，沉淀用丙酮聚合物，并通过1 H NMR中的CD分析它<html> CL 3。 15如果为双键（δ= 4.5-6.0 ppm的）的信号被充分地降低（ 图3），传递给下一个步骤。典型地，该双键的其他质子的积分的比小于1:20（1:83在图3中）。否则，继续反应。 </li><li>添加丙酮（750毫升）到配有磁搅拌棒的4升烧杯中。 </li><li>添加聚合物溶液逐渐丙酮在剧烈搅拌下15分钟。 </li><li>过滤过配备有纸过滤器（413级，直径15厘米）15厘米直径的布氏漏斗的聚合物。 </li><li>用丙酮（每次200毫升）洗涤聚合物的四倍。 </li><li>改变每次洗涤之间的滤纸。 </li><li>干，在室温下真空聚合物7.5克过夜。 </li></ol></li></ol><html> G"/&gt; 图2:粗（顶部）和纯化（底部）NBE（CO 2 H）。1 H NMR光谱。纯化的产物通过简单的蒸馏获得。请注意这是用来评估远藤峰:外型比。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54552/54552fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" src="/files/ftp_upload/54552/54552fig3.jpg" /> 图3:PNBE（乙烯基）（蓝色）和PNBE（环氧基）（红色）的1 H NMR谱。注意比1:乙烯基（δ= 4.5-6.0 ppm的）在PNBE（乙烯基）光谱的积分和其它质子间3。用H 2 O 2的反应后，该比率降低至1:83，从而确认乙烯基的该环氧化已发生。NK"&gt;点击此处查看该图的放大版本。 <img alt="图4" src="/files/ftp_upload/54552/54552fig4.jpg" /> 图4:衰减全反射模式下采集红外光谱PNBE（乙烯）（黑色）和PNBE（环氧树脂）的。将显示PNBE（乙烯）和PNBE（环氧树脂）的特征峰的变焦。 902 -1 992 -1带对应于C = CH外的面外弯曲，而875 -1频带对应于环氧化物环变形。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54552/54552fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

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这里提出的方法简单，易于成规模。因为没有任何纯化接收可以使用的所有化学品。注意，由于在处理和收集期间材料的不可避免的损失进行在较低的比例反应（ 如磅秤≤1G）通常会产生低的产率。 在商业钯化合物与阳离子化剂的反应而原位形成的催化剂。在我们手中，该反应的产率，以及该聚合物的特性（ 如分子量分布）没有改变一个人是否具有良好定义的催化剂开始，如（ɳ3 -烯丙基）的PdS 2 + SBF 6 - （ S =硝基甲烷），或者与原位催化体系。为NBE（乙烯）的聚合，只是催化剂在原位形式目前公知的。我们没有看到有任何反应速度差钯2（DBA）3和Pd（DBA）2，但使用了氯仿加合物，钯2（DBA）3。不建议三氯甲烷 （获得的收益率较低）。聚合反应也略有空气敏感。相比，在手套箱（O 2 &lt;5ppm的）完全进行的反应，我们当反应通过用N 2中，催化剂仍然鼓泡以大致脱气的试剂进行（脱气得到类似的结果在收率和分子量的方面在手套箱被称重）。单体不需要在使用前进行干燥，但不建议有意添加水的存在下，由于水的坐标催化剂和毒物的反应。事实上，该催化剂（ɳ3 -烯丙基）的Pd（OH 2）2 + SBF 6 -被认为是不活动的。 NBE（CO 2 H）的聚合产量停留在45％，由于的形成固体（玻璃化）。残留单体用乙酸乙酯萃取。乙酸乙酯可以从单体通过旋转蒸发来分离和收集的单体可在随后的聚合接合。 内型:在收集的单体外型比距离内切稍有不同:初始单体的外型比。正如我们在先前的工作表明，13的催化剂聚合，但在一个类似的方式收集的单体所得作为初始单体的聚合期间异构内型异构体的外型异构体。 用乙酸乙酯外，不使用任何其它的有机溶剂为PNBE（CO 2 H）的制备中，从DCPD和丙烯酸开始。是可能的取代与水的索氏萃取的乙酸乙酯萃取步骤。这个过程还允许未反应的单体分离，导致反应完全不含溶剂的，但它是乏味（索氏萃取在我们手中历时2天）。 NBE（乙烯）的聚合与产量为0.02摩尔％的催化剂负载的80％进行。为0.01摩尔％的催化剂加载，收率降低到45％。反应停止由于催化剂的分解，并因此，产率是不使用较长的反应时间的改善。期间聚合物的纯化，二氧化硅以去除残留金属加入。与此过程中，聚合物是基本上无银，锑和包含小于15ppm的Pd，如通过ICP测量。 聚合物的环氧化是通过就地形成用H 2 O 2和相应的羧酸过氧和performic酸进行。在过滤步骤（3.1.11和3.1.12）应该没有任何中断尽可能来执行，并尽可能迅速。事实上，在这个阶段中，固体PNE（环氧树脂）与一个大amou接触酸和水的核苷酸，其导致的环氧官能的环开口。为了评估开环官能团的聚合物中的存在，人们可以简单地评估聚合物的二甲基甲酰胺中的溶解度（DMF）中。所述开环聚合物是不溶于DMF中而PNBE（环氧树脂）溶于DMF中。 我们认为这种方法是因为通过官能PNBEs在光致抗蚀剂这是，例如，适于在157纳米光刻法使用的制造中发挥的重要作用显著。 19功能PNBEs也可以用于嵌段共聚物的结构。 20由于其饱和烃骨干，这种聚合物是有趣的微电子低介电材料。 21日前，我们也证明了这些材料导致非常高Tg热固性树脂14以及离聚物与燃料策可能的应用LL膜。 18鉴于可能的应用丰富，这里介绍的方法是进行广泛的社会关注。

降冰片烯，NBE，乙烯和环戊二烯（以双环戊二烯（DCPD）的"裂化"获得的）的狄尔斯-阿德耳加成物，是用任一自由基聚合，1阳离子聚合，2开环复分解聚合3和催化插入容易聚合聚合。 4，5，6，7不同于其他机制，催化插入聚合导致形成非常高的玻璃化转变温度的（T G）聚合物，由此NBE的双环骨架是保守的。各种催化剂，如金属茂催化剂和后过渡金属催化剂，可以使用促进NBE的聚合。 4，5，6， <suP类="外部参照"&gt; 7然而，由于它的低溶解度，并且由于具有非常高的Tg的聚合物的加工有关的困难，所述PNBE均聚物，就我们所知，从未发现的任何用途。 功能冰片烯（PNBEs）已经相当审查的对象为过去20年来，因为他们结合的双环刚性重复单元以及由它们的功能赋予期望的性能赋予高的Tg。 8，9，10 NBE单体选自相当简单和廉价的原料制得，用环戊二烯和官能化亲二烯体之间一步法Diels-Alder反应。然而，Diels-Alder反应导致两种立体异构体， 内和外 ，它们具有非常不同的反应性。 11,12实际上， 内切立体声异构体比外形式减少被动反应，使催化剂失活。 11,12因此，在过去，功能降冰片烯的制备通常需要的内和外的立体异构体的分离，并仅使用外立体异构体。这种分离程序是耗时的，并导致未反应的内切立体不可取废物的积累。 最近我们已经表明，含有两种立体异构体官能NBEs的聚合实际上是可行的。 13我们就此能够制备各种取代的PNBEs的，含有官能团如酯，酸酐，醛，酰亚胺，醇类和双键。由于它们的高的Tg和功能，这些聚合物显示出理想的性质。我们在这里描述的两种方法来制备功能性聚合物。第一个通向水溶性聚合物聚（5-降冰片烯-2-羧酸）的合成中，PNBE（CO 2 H），使用阳离子钯催化剂（ 图1）。 13，14相同的聚合方法可用于制备具有各种挂件官能团，如酯，醇，酰亚胺，溴烷基，醛和酸酐官能PNBEs。在我们手中，这种阳离子钯催化剂不能用于含有侧链双键如5-乙烯基-2-降冰片烯NBEs。在这种情况下，在聚合过程中吊灯双键的一个部分插入导致交联的材料的形成。因此，我们在这里提出专用于形成聚（5-乙烯基-2-降冰片烯），PNBE（乙烯），采用钯2（DBA）3的第二方法:AgSbF 6:PPH 3作为原位催化剂。 14聚合物的侧链乙烯基基团随后进一步环氧化，导致第Ë形成PNBE（环氧树脂）（ 图1）。无论PNBE（CO 2 H）和PNBE（环氧树脂）已发现导致形成热固性树脂的用的Tg高达350℃。 14因此，这里所描述的简单的方法允许人们有效地具有非常高的Tg和具有各种官能团，其可用于多种应用的制备聚合物。 <img alt="图1" src="/files/ftp_upload/54552/54552fig1.jpg" /> 图1:由钯制得的官能PNBEs催化聚合。 （A）PNBE（CO 2 H）的准备，（B）准备PNBE（乙烯）和PNBE（环氧树脂）。虚线键表示内型和外型异构体的混合物。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54552/54552fig1large.jpg" target="_blank">请点击此处查看该网络的放大版本</a>古尔。

<table border="0" cellpadding="0" cellspacing="0" width="945">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">acrylic acid</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td style="width:135px;">147230</td>
			<td style="width:299px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">hydroquinone</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td>H9003</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">dicyclopendadiene</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td align="left">454338</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">palladium allyl dichloride dimer</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td>222380</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">silver hexfluoro antimonate</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td style="width:135px;">227730</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">liquid nitrogen</td>
			<td style="width:241px;">Local Facility</td>
			<td style="width:135px;">NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">ethyl acetate</td>
			<td style="width:241px;">Fischer Scientific</td>
			<td>E14520</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">5-vinyl-2-norbornene</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td style="width:135px;">148679</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">toluene</td>
			<td style="width:241px;">Fischer Scientific</td>
			<td>T290-4</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">palladium dba</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td style="width:135px;">227994</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">triphenyl phosphine</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td style="width:135px;">93090</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">silica gel 40-63 microns</td>
			<td style="width:241px;">Silicycle</td>
			<td style="width:135px;">Siliaflash</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">methanol</td>
			<td style="width:241px;">Fischer Scientific</td>
			<td>BPA412-20</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">dichloromethane</td>
			<td style="width:241px;">EMD Millipore</td>
			<td>DX08311</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">formic acid</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td style="width:135px;">F0507</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">acetic acid</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td>320099</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:271px;">hydrogen peroxide solution</td>
			<td style="width:241px;">Sigma-Aldrich</td>
			<td style="width:135px;">216763</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:271px;">acetone</td>
			<td style="width:241px;">Fischer Scientific</td>
			<td>A18-200</td>
			<td></td>
		</tr>
	</tbody>
</table>

a simple and efficient protocol for the catalytic insertion polymerization of functional norbornenes

降冰片烯可以通过多种机制，包括插入聚合由此双键聚合和单体的双环性质是保守的聚合。所得到的聚合物，降冰片烯，具有非常高的玻璃化转变温度，T g，且有趣的光学和电学性能。然而，功能降冰片烯的由该机构的聚合是通过该内型取代的降冰片烯单体有，在一般情况下，非常低的反应性的事实而复杂化。此外，来自外单体的内型取代的单体的分离是一项乏味的任务。在这里，我们提出了一个简单的协议，用于取代降冰片烯聚合:轴承无论是羧酸或吊坠双键（ 内 约 外 80:20）。该过程不要求两种异构体中分离出来，并用低催化剂负载量（0.01至0.02摩尔％）进行。聚合物轴承挂起蚂蚁双键可以以高收率进一步转化，以得到聚合物轴承环氧侧基。这些简单的程序可以应用于具有各种官能团，如酯，醇，酰亚胺，双键，羧酸，溴烷基，醛和酸酐的制备降冰片烯。

的NBE单体通过的DCPD的简单Diels-Alder反应和合适的亲二烯体，例如丙烯酸（AA）来制备。通常情况下，DCPD被破解的反应之前，产生环戊二烯（CPD）。然后17破获新鲜CPD从事Diels-Alder反应。然而，在该协议中，都伴随执行既裂化和狄尔斯 - 阿德耳步骤，在单罐反应。因此，只要形成的CPD，其与AA反应以得到5-降冰片烯-2-羧酸，NBE（CO 2 H）（ 图1A）。反应后，将粗NBE（CO 2 H）是通过简单蒸馏（ 图2）进行纯化。此过程一直重复以一致的方式的各种亲二烯体的（马来酸酐13，烯丙基溴18，烯丙醇18，1-辛烯18）（高收率，纯化由DIST推理（ 图2）。以丁二烯作为亲二烯体反应没有尝试，由于与丁二烯的操纵相关的固有困难。有趣的是，此反应是无溶剂型。 该聚合物通过催化聚合（ 图1A和1B）得到的干燥粉末的形式下回收。它们由1 H NMR，FTIR光谱和凝胶渗透色谱（GPC）进行分析。聚合物（ 图3）的1 H NMR分析用来诊断剩余溶剂和单体（其显示为尖峰，在对比聚合物的宽共振）的存在。 PNBE（乙烯）（ 图3蓝色）和PNBE（环氧树脂）（ 图3红色）的1 H NMR分析允许PNBE（乙烯基）的环氧化的确认。的确，叔的积分之间的降低率他乙烯基和在PNBE（环氧树脂）谱（1:3至1:83）的其它质子证明该反应（在这种情况下，97％）的优良转化率。的红外光谱也可以用于确认环氧化反应的结果，如在875 -1（ 图4）和的904 992 -1这是在观察到的消失所示的特征峰的幽灵PNBE（乙烯）聚合物。利用GPC用于确认的聚合物的分子量分布。典型Mn为用于PNBE（CO 2 H）和PNBE（环氧树脂）100,000克/摩尔至20,000克/摩尔，以包含在1.5和2.0之间的PDI。

Watch this Scientific Journal Video about A Simple and Efficient Protocol for the Catalytic Insertion Polymerization of Functional Norbornenes at JoVE.com

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

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.

功能性降冰片烯的催化聚合插入一种简单高效的协议

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

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10.2K 次观看.  Université de Sherbrooke. 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. 

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

A Simple and Rapid Protocol for Measuring Neutral Lipids in Algal Cells Using Fluorescence

Algae are considered excellent candidates for renewable fuel sources due to their natural lipid storage capabilities. Robust monitoring of algal fermentation processes and screening for new oil-rich strains requires a fast and reliable protocol for determination of intracellular lipid content. Current practices rely largely on gravimetric methods to determine oil content, techniques developed decades ago that are time consuming and require large sample volumes. In this paper, Nile Red, a fluorescent dye that has been used to identify the presence of lipid bodies in numerous types of organisms, is incorporated into a simple, fast, and reliable protocol for measuring the neutral lipid content of Auxenochlorella protothecoides, a green alga. The method uses ethanol, a relatively mild solvent, to permeabilize the cell membrane before staining and a 96 well micro-plate to increase sample capacity during fluorescence intensity measurements. It has been designed with the specific application of monitoring bioprocess performance. Previously dried samples or live samples from a growing culture can be used in the assay.

A simple protocol to determine the neutral lipid content of algal cells using a Nile Red staining procedure is described. This time-saving technique offers an alternative to traditional gravimetric-based lipid quantification protocols. It has been designed for the specific application of monitoring bioprocess performance.

一种简单快速的协议用荧光测量中性脂肪在藻细胞

Algae are considered excellent candidates for renewable fuel sources due to their natural lipid storage capabilities. Robust monitoring of algal ...

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化学

Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica

As a promising catalytically active nano reactor, gold nanoparticles intercalated in mesoporous silica (GMS) were successfully synthesized and properties of the materials were investigated. We used a one pot sol-gel approach to intercalate gold nano particles in the walls of mesoporous silica. To start with the synthesis, P123 was used as template to form micelles. Then TESPTS was used as a surface modification agent to intercalate gold nano particles. Following this process, TEOS was added in as a silica source which underwent a polymerization process in acid environment. After hydrothermal processing and calcination, the final product was acquired. Several techniques were utilized to characterize the porosity, morphology and structure of the gold intercalated mesoporous silica. The results showed a stable structure of mesoporous silica after gold intercalation. Through the oxidation of benzyl alcohol as a benchmark reaction, the GMS materials showed high selectivity and recyclability.

Here, we present a protocol with a sol-gel process to synthesize gold intercalated in the walls of mesoporous materials (GMS), which is confirmed to possess a mesoporous matrix with gold intercalated in the walls imparting great stability and recyclability.

合成和金插在介孔二氧化硅的墙壁催化性能

As a promising catalytically active nano reactor, gold nanoparticles intercalated in mesoporous silica (GMS) were successfully synthesized and properties ...

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.

通过RAFT控制聚合轻便和高效制备三组分荧光Glycopolymers

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.

乙烯聚合中使用并联电抗器的压力和链转移聚合的动力学分析

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

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of trifluoromethoxylated aromatic compounds remains a formidable challenge in organic synthesis. Conventional approaches often suffer from poor substrate scope, or require use of highly toxic, difficult-to-handle, and/or thermally labile reagents. Herein, we report a user-friendly protocol for the synthesis of methyl 4-acetamido-3-(trifluoromethoxy)benzoate using 1-trifluoromethyl-1,2-benziodoxol-3(1H)-one (Togni reagent II). Treating methyl 4-(N-hydroxyacetamido)benzoate (1a) with Togni reagent II in the presence of a catalytic amount of cesium carbonate (Cs2CO3) in chloroform at RT afforded methyl 4-(N-(trifluoromethoxy)acetamido)benzoate (2a). This intermediate was then converted to the final product methyl 4-acetamido-3-(trifluoromethoxy)benzoate (3a) in nitromethane at 120 &#176;C. This procedure is general and can be applied to the synthesis of a broad spectrum of ortho-trifluoromethoxylated aniline derivatives, which could serve as useful synthetic building blocks for the discovery and development of new pharmaceuticals, agrochemicals, and functional materials.

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

An operationally simple procedure for the synthesis of ortho-trifluoromethoxylated aniline derivatives via a two-step sequence of O-trifluoromethylation of N-aryl-N-hydroxyacetamide followed by thermally induced intramolecular OCF3-migration is reported.

协议的合成<em&gt;邻</em&gt; -trifluoromethoxylated苯胺类化合物

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of ...

A Protocol for the Production of Gliadin-cyanoacrylate Nanoparticles for Hydrophilic Coating

This article presents a protocol for the production of protein-based nanoparticles that changes the hydrophobic surface to hydrophilic by a simple spray coating. These nanoparticles are produced by the polymerization reaction of alkyl cyanoacrylate on the surface of cereal protein (gliadin) molecules. Alkyl cyanoacrylate is a monomer that instantly polymerizes at RT when it is applied to the surface of materials. Its polymerization reaction is initiated by the trace amounts of weakly basic or nucleophilic species on the surface, including moisture. Once polymerized, the polymerized alkyl cyanoacrylates show a strong affinity with the object materials because nitrile groups are in the backbone of poly (alkyl cyanoacrylate). Proteins also work as initiator for this polymerization because they contain amine groups that can initiate the polymerization of cyanoacrylate. If aggregated protein is used as an initiator, protein aggregate is surrounded by the hydrophobic poly(alkyl cyanoacrylate) chains after the polymerization reaction of alkyl cyanoacrylate. By controlling the experimental condition, particles in the nanometer range are produced. The produced nanoparticles readily adsorb to the surface of most materials including glass, metals, plastics, wood, leather, and fabrics. When the surface of a material is sprayed with the produced nanoparticle suspension and rinsed with water, the micellar structure of nanoparticle changes its conformation, and the hydrophilic proteins are exposed to the air. As a result, the nanoparticle-coated surface changes to hydrophilic.

This article presents a protocol for the production of protein-based nanoparticles that changes the hydrophobic surface to hydrophilic. The produced nanoparticle is an assembly of gliadin-cyanoacrylate diblock copolymers. Spray coating with the produced nanoparticle changes the surface of target material to a hydrophilic surface.

一种醇溶蛋白氰基丙烯酸酯纳米粒子为亲水涂料生产协议

This article presents a protocol for the production of protein-based nanoparticles that changes the hydrophobic surface to hydrophilic by a simple spray ...

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.

使用Photoredox催化剂蠕虫状胶束的简便合成可见光介导的分散聚合

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

An Optimized Protocol for the Efficient Radiolabeling of Gold Nanoparticles by Using a 125I-labeled Azide Prosthetic Group

Here, we demonstrate a detailed protocol for the radiosynthesis of a 125I-labeled azide prosthetic group and its application to the efficient radiolabeling of DBCO-group-functionalized gold nanoparticles using a copper-free click reaction. Radioiodination of the stannylated precursor (2) was carried out by using [125I]NaI and chloramine T as an oxidant at room temperature for 15 min. After HPLC purification of the crude product, the purified 125I-labeled azide (1) was obtained with high radiochemical yield (75 &plusmn; 10%, n = 8) and excellent radiochemical purity (&gt;99%). For the synthesis of radiolabeled 13-nm-sized gold nanoparticles, the DBCO-functionalized gold nanoparticles (3) were prepared by using a thiolated polyethylene glycol polymer. A copper-free click reaction between 1 and 3 gave the 125I-labeled gold nanoparticles (4) with more than 95% of radiochemical yield as determined by radio-thin-layer chromatography (radio-TLC). These results clearly indicate that the present radiolabeling method using a strain-promoted copper-free click reaction will be useful for the efficient and convenient radiolabeling of DBCO-group-containing nanomaterials.

An Optimized Protocol for the Efficient Radiolabeling of Gold Nanoparticles by Using a 125I-labeled Azide Prosthetic Group

A detailed procedure for the synthesis of a 125I-labeled azide and the radiolabeling of dibenzocyclooctyne (DBCO)-group-conjugated, 13-nm-sized gold nanoparticles using a copper-free click reaction is described.

一个优化的协议通过使用金纳米粒子的放射性标记效率<sup&gt; 125</sup&gt;我标记的叠氮辅基

Here, we demonstrate a detailed protocol for the radiosynthesis of a 125I-labeled azide prosthetic group and its application to the efficient ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

化学沉淀法合成铌2O5改性高比表面积镍催化剂

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three preparation methods are described: (a) the incorporation of metal salts into silica or alumina wet gels using an impregnation method; (b) the incorporation of metal salts into alumina wet gels using a co-precursor method; and (c) the addition of metal nanoparticles directly into a silica aerogel precursor mixture. The methods utilize a hydraulic hot press, which allows for rapid (&#60;6 h) supercritical extraction and results in aerogels of low density (0.10 g/mL) and high surface area (200-800 m2/g). While the work presented here focuses on the use of copper salts and copper nanoparticles, the approach can be implemented using other metal salts and nanoparticles. A protocol for testing the three-way catalytic ability of these aerogels for automotive pollution mitigation is also presented. This technique uses custom-built equipment, the Union Catalytic Testbed (UCAT), in which a simulated exhaust mixture is passed over an aerogel sample at a controlled temperature and flow rate. The system is capable of measuring the ability of the catalytic aerogels, under both oxidizing and reducing conditions, to convert CO, NO and unburned hydrocarbons (HCs) to less harmful species (CO2, H2O and N2). Example catalytic results are presented for the aerogels described.

Here we present protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms. Methods for preparing materials using copper salts and copper-containing nanoparticles are featured. Catalytic testing protocols demonstrate the effectiveness of these aerogels for three-way catalysis applications.

快速超临界萃取制备催化气凝胶的制备与试验研究

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...