Microwave Reactor and Raman Spectrometer for In Situ Reaction Analysis

所要求的带有拉曼光谱仪和自动取样器的微波反应堆将是执行和分析高温和高压反应的关键基础设施。这种独特的仪器组合于2019年刚刚上市，并提供了一种新的、独特的工具来执行微波反应的在线监测。通过允许反应动力学和对关键反应中间体的观察，它将提供一个重要的新工具来促进反应机理的确定，这是开发新的反应性和优化新的化学转化的关键参数。该设备将提供加拿大独一无二的测量能力，并将使研究人员能够在合成化学方面取得进展，否则他们将无法获得这些进展。*申请人实验室的反应通常在惰性气氛下进行，以消除外来氧气、水分或防止挥发性反应物逃逸。然而，由于缺乏可用于原位分析的方法，对这些反应的研究变得混乱。遗憾的是，包括核磁共振和反应红外在内的其他反应监测方法不适用于高温高压反应的研究，也不能用于分析敏感的有机金属催化剂的反应。因此，在分子水平上研究新发现的反应可能非常具有挑战性，甚至是不可能的。这些限制的影响可能导致：(I)效率较低的催化系统的开发，(Ii)无法根据反应结果起草和验证准确的假设，以及(Iii)延迟对科学期刊上的发表、与学术和工业合作伙伴的合作以及该领域的基本进展产生负面影响。由于Anton-Paar在拉曼光谱和微波反应器方面的专业知识相结合，现在可以通过插入微波反应腔中的光纤探头从密封管外部获得拉曼测量。微波炉将配备自动取样器，使反应筛选自动化，并方便HQP培训。因此，由于反应可以全天候进行，因此生产率将大大提高。该仪器将为使用微波反应堆的约60名HQP提供新的资源，为其他人批量执行反应动力学提供新的能力，HQP培训计划涉及一个小型、多样化的团队，以促进培训、反应设置和分析。这将促进在渥太华内部采用简化反应发现和优化的技术，并使外部用户能够访问这一新功能。

The requested microwave reactor with Raman spectrometer and autosampler will be critical piece of infrastructure to execute and analyze high-temperature and high-pressure reactions. This unique combination of instruments just became commercially available in 2019 and provides a new, unique tool to perform in-line monitoring of microwave reactions. By allowing reaction kinetics and the observation of key reaction intermediates, it will provide a crucial new tool to facilitate the determination of reaction mechanisms, a key parameter for the development of new reactivity and optimization of novel chemical transformations. This equipment will provide measurement capabilities unique in Canada and will enable researchers to make advances in synthetic chemistry that otherwise would not be accessible to them. ******Reactions in the applicants' laboratories are routinely performed under inert atmosphere to eliminate exogenous oxygen, moisture or to prevent volatile reactants from escaping. However, the study of these reactions is obfuscated by the lack of available methods for in situ analysis. Other methods to perform reaction monitoring, including NMR and ReactIR are unfortunately not suitable to the study of high-temperature and high-pressure reactions, and also cannot be used to analyze reactions of sensitive organometallic catalysts. Consequently, the study of newly discovered reactions at the molecular level can be exceptionally challenging or impossible. The impact of these limitations can lead to: (i) the development of less efficacious catalytic systems, (ii) the inability to draft and validate accurate hypotheses based on reaction outcomes, and (iii) delays that negatively impact publication in scientific journals, collaborations with academic and industrial partners and fundamental advances in the field.******In contrast, acquisition of this instrument will have immediate impact on the applicants' ability to analyze high-temperature and high-pressure reactions. Due to the combination of Anton-Paar's expertise in Raman spectroscopy and microwave reactors, Raman measurements can now be obtained from outside the sealed tube via a fibre optic probe inserted into the microwave reaction cavity. The microwave will be equipped with an auto-sampler to make reaction screening autonomous and facilitate HQP training. Therefore, productivity would be greatly enhanced as reactions could be run on a nearly 24/7 basis. This instrument will provide a new resource to the ca. 60 HQP that use microwave reactors, a new capability to perform reaction kinetics in batch for others, and the HQP training plan involves a small, diverse team to facilitate training, reaction setup and analysis. This will facilitate adoption of a technology streamlining reaction discovery and optimization within uOttawa, and enable outside users to access this new capability.*****