As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1003711-43-0, name is 2-Bromo-5-hydroxy-3-methylpyridine, molecular formula is C6H6BrNO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. HPLC of Formula: C6H6BrNO
6-Bromo-5-methylpyridin-3-ol (10.4 g, 55.3 mmol) and NCS (8.12 g, 60.8 mmol) in Nu,Nu-dimethylformamide (DMF) (150 mL) were heated at 80 C for 2 hours. The mixture was allowed to cool to room temperature, quenched with brine, and extracted 3 times with ethyl acetate. The combined organic layers were washed with 5% lithium chloride, washed with brine, dried over sodium sulfate, and concentrated. The residue was purified by silica chromatography eluting with a gradient of 0% to 50% ethyl acetate in hexanes. Fractions were concentrated to give 6-bromo-2-chloro-5-methylpyridin-3-ol (7.85 g, 35.3 mmol, 63.8 % yield) as a white powder. LCMS(ES+)(m/z) : 222, 224, 226 (M+1 ).
With the rapid development of chemical substances, we look forward to future research findings about 1003711-43-0.
Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; CATALANO, John G.; CHONG, Pek Yoke; DICKSON, Hamilton D.; LEIVERS, Martin R.; WEATHERHEAD, Jason Gordon; (186 pag.)WO2019/69293; (2019); A1;,
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