Electric Literature of 1450-93-7,Some common heterocyclic compound, 1450-93-7, name is 1H-imidazol-2-amine sulfate(2:1), molecular formula is C6H12N6O4S, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Synthesis of (E)-4-((1H-imidazol-2-yl)diazenyl)-1-methyl-1H-pyrazol-5-amine Concentrated HCl (17.16 mL, 206 mmol) and 1H-imidazol-2-aminium sulfate (6.67 g, 25.1 mmol) were added to a 150 mL Erlenmeyer flask and cooled in ice/methanol bath to <0 C. Sodium nitrite (3.55 g, 51.48 mmol) is dissolved in ca. 20 mL of water and added dropwise to the solution above keeping the temperature below 5 C. In a separate flask sodium carbonate (27.2 g, 257 mmol) is dissolved in 200 mL of water. 1-Methyl-1H-pyrazol-5-amine (5 g, 51.48 mmol) is added. Upon cooling and stirring the solution became slushy. The 2-aminoimidazole containing solution is added to the 1-methyl-5-aminopyrazole solution, keeping the temperature below 5 C. Following complete addition the reaction mixture is kept cold and stirred for ca. 1 hour. Ethyl acetate (1 L) is added to the reaction mixture and the mixture is transferred to 2 L separatory funnel. The ethyl acetate is collected, and the aqueous phase is extracted twice more with ethyl acetate (2*1 L). The extracts were combined and evaporated providing 5.0 g of a black semi-solid. The crude (E)-4-((1H-imidizol-2-yl)diazenyl)-1-methyl-1H-pyrazol-5-amine is purified by column chromatography.
The synthetic route of 1450-93-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; NOXELL COPRORATION; MURPHY, Bryan Patrick; ZHANG, Guiru; GARRETT, Garry Steven; (41 pag.)US2018/79907; (2018); A1;,
Imidazole – Wikipedia,
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