Some common heterocyclic compound, 127107-23-7, name is 1-Methyl-1H-pyrazol-4-amine hydrochloride, molecular formula is C4H8ClN3, 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. category: pyrazoles-derivatives
Into a 25 mL round-bottom flask, were placed intermediate 44.3 (300 mg, 0.74 mmol, 1.00 equiv), 1-methyl-1H-pyrazol-4-amine hydrochloride (119 mg, 0.89 mmol, 1.20 equiv), hydrogen chloride in dioxane (0.5 mL) and n-BuOH (5 mL). The reaction was stirred for 12 h at 110 C. Upon completion of the reaction resulting mixture was concentrated under vacuum. The solution was adjusted to pH 9-10 with sodium hydroxide (2M) and resulting solids were collected by filtration. The crude product was purified by recrystallization from methanol to furnish 208.8 mg (61%) of compound 1-45 as a yellow solid. LCMS (ES, mlz): 465.4[M+H] ?H NMR (300MHz, CD3OD): 7.86 (1H, s), 7.54 (1H, s), 6.75-7.11 (1H, t), 4.05 (1H, s), 3.85 (3H, s), 3.78 (4H, t), 2.60 (4H, s), 2.08-2.32 (5H, m), 1.29-1.47 (4H, m).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 127107-23-7, its application will become more common.
Reference:
Patent; NIMBUS IRIS, INC.; ROMERO, Donna L.; MASSE, Craig E.; ROBINSON, Shaughnessy; GREENWOOD, Jeremy Robert; HARRIMAN, Geraldine; WO2015/48281; (2015); A1;,
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