Electric Literature of 32673-41-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 32673-41-9 name is 4-Imidazolemethanol hydrochloride, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
538 mg starting material (4 mmol) was dissolved in ~ 4 ml methanol and 500 mg NaHCO3 (6 mmol) was added. The tube was occasionally stirred for 60 min, alternatively at 4 C and at warm water temperature. CO2 was allowed to escape from the glass tube. The mix was divided across several Eppendorf tubes and subjected to Speedvac treatment for 1 hour. Residues were white solids with light-yellow sirupy liquids. Chloroform/methanol mix 1:1 was added to the tubes with subsequent gentle warming and stirring. NaHCO3 was separated by centrifugation of the combined fractions at 3500 rpm for 5 min. Clear supernatant was kept overnight at -20 C to allow the precipitation of additional NaHCO3. Then, the solution was cleared by filtration and evaporated to dryness with a Rotavapor device. The residue was taken up in 20 ml dioxane with magnetic stirring and 4.4 mg MnO2 (activated; for synthesis) was added in the same flask. The residue may not have been dissolved completely in first instantion. The mix was refluxed for 2 hours on a paraffin oil bath. The warm solution was filtered and MnO2 was washed once with warm dioxane. Dioxane was evaporated with the Rotavapor yielding a white and yellow fine cristalline solid. Crystallization was carried out in methanol repeated times. Small volumes of methanol were required, because the residue dissolved well in methanol
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Imidazolemethanol hydrochloride, and friends who are interested can also refer to it.
Reference:
Patent; Academisch Ziekenhuis bij de Universiteit van Amsterdam; EP1196129; (2005); B1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem