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 3314-30-5 as follows. 3314-30-5
To a mixture of X4-011-1 (2 g, 12.4 mmol) and 1H-benzo[d]imidazole-2- carbaldehyde (2.72 g, 18.6 mmol) in MeOH (60 ml) was added a solution of NaOH (992 mg, 24.8 mmol) in H20 (4 ml) at 0 ¡ãC and the mixture was stirred at room temperature for 3 h. The solution was adjusted pH to 8 with 35percent HC1 aq., dried over anhydrous Na2SO4, filtered and concentrated in vacuum. The residue was purified by column chromatography to give X4-011-2 (2.7 g, 75.2 percent yield) as a yellow solid. LCMS (Agilent LCMS 1200-6110, Column: Waters XBridge C18 (50 mm*4.6 mm*3.5 jim); Column Temperature: 40 ¡ãC; Flow Rate: 2.0 mL/min; Mobile Phase: from 95percent [0.05percent aq. TFA] and 5percent [CH3CN + 0.05percent TFA] to 0percent [0.05percent aq. TFA] and 100percent [CH3CN + 0.05 percent TFA] in 1.6 mm, then under this condition for 1.4 mm, finally changed to 95percent [0.05percent aq. TFA] and 5percent [CH3CN + 0.05percent TFA] in 0.05 mm and under this condition for 0.7 mi. Purity: 99percent; Rt = 1.32 mm; MS Calcd.: 289.1; MS Found: 290.1 [M+H].
According to the analysis of related databases, 3314-30-5, the application of this compound in the production field has become more and more popular.
Reference:
Patent; X4 PHARMACEUTICALS, INC.; BOURQUE, Elyse Marie Josee; SKERLJ, Renato; (279 pag.)WO2017/223229; (2017); A1;,
Imidazole – Wikipedia,
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