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 1243204-92-3 as follows. Quality Control of 3-Methoxy-4-(4-methyl-1H-imidazol-1-yl)benzonitrile
[0428] To a stirred solution of 3-methoxy-4-(4-methyl-1H-imidazol-1-yl) benzonitrile (450 mg, 2 mmol) in MeOH (23 mL) at room temperature under an argon atmosphere were added hydroxyl amine hydrochloride (230 mg, 2 mmol) and sodium bicarbonate (230 mg, 3 mmol). The reaction mixture was stirred at 85 C for 3 h. After consumption of starting material (by TLC), the volatiles were evaporated in vacuo. The residue was diluted with ice cold water (50 mL), stirred for 10 mm, to obtain the solid. The solid was collected by filtration and dried in vacuo to obtain (Z)-iV-hydroxy-3-methoxy-4-(4-methyl-1H-imidazol-1- yl) benzimidamide (450 mg, 88%) as an off-white solid.?H NMR (DMSO-d6, 500 MHz): 9.73 (s, 1H), 7.79 (s, 1H), 7.47 (s, 1H), 7.37 (s, 2H), 5.92 (s, 2H), 3.82 (s, 3H), 2.15 (s, 3H); LCMS: 92.4%; 247 (M+1); (column; X-select CSH C-18 (50 x 3.0 mm, 2.7 tim); RT 2.06 mm; mobile phase: 2.5mM NH400CH in water+5% ACN:ACN+5% 2.5mM NH400CH in water; T/B%: 0.01/5, 0.5/5, 3/100, 5/100; flow rate: 1.2 mL/min) (Gradient); TLC: 3% MeOH/CH2C12 (R1: 0.3).
According to the analysis of related databases, 1243204-92-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; FORUM PHARMACEUTICALS INC.; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; HARRISON, Bryce, Alden; (273 pag.)WO2017/31325; (2017); A1;,
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