During a 2-week practical course, students will be introduced to the preparation, manipulation and characterization of air- and temperature-sensitive compounds by using synthesis in the glovebox and Schlenk technique. They will be trained in purifying solvents for sensitive transformations, working with argon/vacuum manifold, using Schlenk flasks, operating glovebox, performing filtration, distillation, sublimation and/or crystallization under strict inert atmosphere, preparing samples and making routine characterizations of prepared products. The laboratory will be carried out at the Institute of Inorganic Chemistry (IIC), Czech Academy of Science. The practical content listed below is just a guideline for the possible work to the done - laboratory tasks will be updated annually according to the latest trends and challenges. Practicals will also reflect the student's research topic with an emphasis on individualization. Motivation Organic synthesis is an important tool in modern science and industry. It enables the preparation of various compounds like pharmaceuticals, functional materials, agrochemicals etc. The laboratory will focus on advanced techniques of preparation and isolation of reactive compounds. Students will learn advanced laboratory techniques of how to isolate reaction products in a controlled environment. The goal is to deepen skills and gain experience with a modern glovebox and Schlenk-line synthesis. Objectives The main goal is to introduce students to the advanced techniques of organic synthesis, and expand their experience with glovebox, Schlenk line and manipulating air-sensitive molecules. Firstly, students will learn how to operate argon-filled glovebox, prepare and handle Schlenk glassware, how to dry solvents from residual moisture and other impurities and how to set up a chemical reaction with strict exclusion of air. Furthermore, they will get experience with general purification methods such as cannula filtration, distillation and sublimation under controlled conditions and isolation and characterization of reaction products. The specific set of reactions will be customized to the previous synthetic experience of students. Anticipated topics include the preparation and isolation of free N-heterocyclic carbene, transition metal-catalysed reactions (Suzuki-Miyaura cross-coupling), manipulation of organometallic reagents (such as butyllithium) and the synthesis of boron-containing cationic compounds. An important aspect of the practical will be the isolation and characterization of prepared compounds, particularly by using multinuclear Nuclear Magnetic Resonance (NMR). Students will acquire experience in the preparation and measurement of samples sensitive to the atmosphere and further enhance their NMR skills. The IIC is equipped with argon-filled glovebox Inert PURE-Lab, several Schlenk-lines and all necessary equipment. Characterization of prepared compounds will be performed primarily on JEOL 600 NMR spectrometer. Acquired skills During the course, students will gain proficiency in handling air-sensitive molecules, and mastering the operation of a glovebox and Schlenk line. They will learn to adeptly prepare and conduct reactions involving sensitive substances (such as free carbenes, organolithium reagents etc.), expanding their expertise in maintaining controlled environments. Furthermore, students will develop the ability to characterize compounds by using advanced techniques like multinuclear NMR, enabling them to elucidate complex molecular structures. This hands-on experience will empower them to confidently navigate challenges associated with sensitive compounds and controlled atmospheres, preparing them for success in intricate organic synthesis endeavours.
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