Synthetic Route of 152628-03-0, These common heterocyclic compound, 152628-03-0, name is 4-Methyl-2-propyl-1H-benzo[d]imidazole-6-carboxylic acid, its 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.
A mixture of 15 g of 4-methyl-2-propyl-1H-benzimidazole-6-carboxylic acid and 100 mL of sulfonyl chloride was allowed to stand at room temperature overnight, heated and stirred at an oil-bath temperature of 80C for five hours, then combined with 0.1 mL of dimethylformamide and again heated and stirred at 80C for five hours. After the sulfonyl chloride had been distilled off under reduced pressure, the residue was combined with 300 mL of dry dimethylformamide and 15 g of methylamine hydrochloride, then 40 g of triethylamine were dropped in while cooling with ice. The residue resulting from stirring at room temperature for two days, then distilling off the solvent was combined with ethyl acetate and physiological saline, and the ethyl acetate layer was separated. The ethyl acetate layer was washed with saturated physiological saline, then dried over anhydrous sodium sulfate. The residue resulting from distilling off the solvent was refined by silica gel column chromatography (elution solvent: ethyl acetate/methanol = 10/1) to give 4.4 g of the intended compound as a white solid. Mass spectrum: 232 (M+1)+.
The synthetic route of 152628-03-0 has been constantly updated, and we look forward to future research findings.