55589-47-4, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.55589-47-4, name is 3-Methylpicolinaldehyde, molecular formula is C7H7NO, molecular weight is 121.14, as common compound, the synthetic route is as follows.
To a solution of X4-012-3 (4.0 g, 21.5 mmol), L-proline (1.0 g, 8.7 mmol) and 3-methylpicolinaldehyde (3.4 g, 28.0 mmol) in MeOH (200.0 mL) was added aq. methanamine (6 mL, 40percent). The solution was stirred at room temperature overnight. The solvent was removed under reduced pressure and purified by column chromatography to give X4-012-4 (4.1 g, 59.6 percent yield) as an orange solid. The structure was confirmed by H-HNOESY. LCMS (Agilent LCMS 1200-6120, Column: Waters X-Bridge C18 (50 mm*4.6 mm*3.5 iim); Column Temperature: 40 ¡ãC; Flow Rate: 2.0 mL/min; Mobile Phase: from 90percent [(total 10 mM AcONH4) water/CH3CN = 9/1 (v/v)] and 10percent [(total 10 mM AcONH4) water/CH3CN = 1/9 (v/v)] to 10percent [(total 10 mM AcONH4) water/CH3CN = 9/1 (v/v)] and 90percent [(total 10 mM AcONH4) water/CH3CN = 1/9 (v/v)] over 1.6 mm, then held under this condition for 2.4 mm, finally changed to 90percent [(total 10 mM AcONH4) water/CH3CN = 9/1 (v/v)] and 10percent [(total 10 mM AcONH4) water/CH3CN = 1/9 (v/v)] over 0.1 mm and held under this condition for 0.7 mi. Purity: 74.83 percent. Rt = 1.49 mm; MS Calcd.: 320.1; MS Found: 321.2 [M + H], MS Found:353.3 [M+MeOH].
Statistics shows that 55589-47-4 is playing an increasingly important role. we look forward to future research findings about 3-Methylpicolinaldehyde.
Reference:
Patent; X4 PHARMACEUTICALS, INC.; BOURQUE, Elyse Marie Josee; SKERLJ, Renato; (279 pag.)WO2017/223229; (2017); A1;,
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