Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 15128-89-9, name is 3-Hydroxy-4-methyl-2-nitropyridine. A new synthetic method of this compound is introduced below., category: pyridine-derivatives
To a solution of 4-methyl-2-nitropyridin-3-ol (4.85 g) in methanol (90 mL) was added 28% sodium methoxide solution in methanol (6.3 mL) . The solution was stirred at room temperature for 15 min and then cooled with an ice-bath. A solution of bromine (1.6 mL) in methanol (15 mL) was added dropwise, and the reaction mixture was stirred at 00C for 2 hr and concentrated to give crude 6-bromo-4-methyl-2- nitropyridin-3-ol, which was used for the next step without further purification. To a mixture of crude 6-bromo-4- methyl-2-nitropyridin-3-ol and potassium carbonate (8.70 g) in acetone (70 mL) was added ethyl bromoacetate (3.5 mL) . The mixture was refluxed for 15 hr and the solvent was evaporated. DMSO (50 mL) , potassium carbonate (5.00 g) and ethyl bromoacetate (1.5 mL) were additionally added, and the mixture was stirred at room temperature for 60 hr, poured into water and extracted with ethyl acetate. The extract was washed with 5% aqueous Na2S2O3, water and saturated aqueous NaHCO3, dried over MgSO and concentrated. The residue was chromatographed on silica gel using n-
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Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2007/77961; (2007); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem