9/1/21 News Continuously updated synthesis method about 51605-32-4

According to the analysis of related databases, 51605-32-4, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 51605-32-4 as follows. COA of Formula: C7H10N2O2

(5-Methylimidazol-4-yl)methylchloride hydrochloride (14) A paste of ethyl 4-methyl-5-imidazolecarboxylate (37.5 g, 0.243 mol) and a little dry THF was added in portions to a stirred suspension of LiAlH4 (12.0 g, 0.316 mol) in 1.0 L of dry THF under a flow of nitrogen. After refluxing for 4 h, the suspension was cooled in an ice-water bath and the excess LiAlH4 destroyed with successive additions of 12 mL of H2 O, 12 mL of 15percent NaOH, and 45 mL of H2 O. The white suspension was brought to room temperature (2 h) and filtered. After collecting the precipitate, it was digested in hot THF (500 mL), cooled, and filtered again. The total THF filtrate was concentrated in vacuo, the residual orange oil was dissolved in a minimum amount of EtOH, and 500 mL of hot EtOAc:Et2 O (3:2) was added. The solution was chilled yielding 15.0 g (55percent) of (5-methylimidazol-4-yl)methanol as white prisms: mp 138° (lit. 138°). This material (9.6 g, 0.086 mol) was dissolved in 50 mL of conc HCl and heated on a steam bath for 30 min. The acidic mixture was concentrated in vacuo to dryness and the solid dissolved in a minimum amount of EtOH. With the addition of a little dry Et2 O, 14 (8.5 g, 67percent) precipitated as a white powder: mp 236°-237° (lit. 222°).

According to the analysis of related databases, 51605-32-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Research Corporation; US4432983; (1984); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem