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Crystals formed after the evaporation of the solvent from a perfectly pure product.
It is adorable to see that a transparent liquid turns into a crystalline mass while standing on the lab bench. It is great to see a spot or spots where crystals start to form and they grow til any remaining compound is on the wall of the flask.
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Preparation of a 2-bromobenzoic acid derivative from an anthranilic acid derivative using the Sandmeyer reaction.
The Sandmeyer reaction is a chemical reaction used to synthesize aryl halides from aryl diazonium salts. It is named after the Swiss chemist Traugott Sandmeyer. The reaction is a method for substitution of an aromatic amino group via preparation of its diazonium salt followed by its displacement with a nucleophile, often catalyzed by copper(I) salts.
ArN2+ + CuBr → ArBr + N2 + Cu+
On the picture and gifs the solution of copper(I)-bromide is being added to the chilled, freshly prepared diazonium salt solution and as the the two reactants mix, almost instantly nitrogen gas forms and the reaction starts.
Interesting thing is that the copper(I)-bromide is a colorless, nearly insoluble solid when pure, however when mixed with hydrobromic acid it dissolved rapidly and gives a deep purple colored solution as seen on the pictures.
Performing reactions on small scale, on low temperature (in this case −78.5 °C , (194.65 K; −109.3 °F) using a Dry ice/acetone cooling bath.
The reactions were performed to check which base is the ideal for an organic transformation. And just as usual, 1 from the 3 reaction gave the product, and in even this reaction a low yield was obtained. But at least now we know that the transformation could be performed, since it was not yet described anywhere.
