Summary of experimental results and procedures for three organic chemistry experiments: synthesis of Diantilis derivatives, Diels-Alder reaction, and Wittig reaction.
Extract
[...] The IR spectra: The compound Méthyl Diantilis (and its derivatives) is often synthesized for the creation of perfumes (sweet scent/vanilla). Cf. https://shop.perfumersapprentice.com/p-6165-methyl-diantilis-givaudan.aspx. Diels Alder Reaction: Different CCMs: In reference thiobenzamide in dichloromethane. Cs: co spot 1 In synthesized heterodiene we see that there is no longer the starting product (thiobenzamide). In initial product (heterodiene, red powder that we have dissolved in acetone). Cs: 1 In final product before synthesizing the thiazine, a little of the initial product remains so let the reflux continue a bit and redo a CCM. [...]
[...] This component will therefore influence the critical view of the results. This component impacts the experiment from start to finish; indeed, the student must constantly be protected (lab coat and goggles), especially in the case of projections (liquid/liquid extraction of Diels-Alder, acid/base reaction). In addition, during the handling of the products, the wearing of gloves is essential (use of corrosive products such as sodium or ethanoic acid used in the synthesis experiment of the Diantilis d'éthyl : from which the interest of knowing the properties of the reactants before coming to TP). [...]
[...] For the three experiments, the use of a rotavapor will be necessary at the end when we have obtained our final product to evaporate the remaining solvents, this in order to obtain the most pure product possible. Here, the component also impacts the hygiene and safety rules (use of reagents) and the respect of the protocol (the synthesis of the requested molecule within the given time can only be done from an adapted experimental strategy). Part Respect of hygiene, safety, deontology rules: This component concerns the protection of oneself, others, and the environment. As well as respect for the laboratory and deontological rules, i.e., the student should not adjust their results according to what they expected. [...]
[...] For the three reactions, we will use at least once a reflux apparatus (Cf [...]
[...] For filtrations, we will use a Buchner assembly (Cf Organic Experimental Chemistry - Hermann chapter II 5). This type of assembly is adapted to our objectives as it allows us to isolate the expected products. In the reaction of Wittig, we have used this filtration several times: after 2 hours of reflux, we filter on Buchner with acetone (and not with water because it is used in the next step). We obtain a phosphonium salt in powder form, we add to this salt water + benzaldehyde) sodium with a dropping funnel (to not add the sodium too quickly because it is very reactive). [...]
