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. 19230-57-0, name is 2-Bromo-3-methylpyridine 1-oxide, 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. COA of Formula: C6H6BrNO
To a stirred solution of 2-bromo-3-methyl pyridine-1-oxide (25g) and pyridine (42g) in acetonitrile (250mL) at about 70C, was added a solution of trifluoromethanesulfonic anhydride (55g) in acetonitrile (5OmL). The reaction mixture was stirred for about lh atabout the same temperature. The mixture was cooled to about 10C to about 15C and ethanolamine (80.52g) was added to it. The reaction mixture was stirred for about 3h at about room temperature and water and ethyl acetate were added to it. The two layers were separated and the organic layer was washed with saturated brine solution, dried and concentrated under reduced pressure at about 40C. The residue was purified by columnchromatography (15-20% ethyl acetate in hexane). Yield: 4g (16%)?H NIVIR (300IVIHz, CDC13): oe 7.26-7.24 (d,J8.lOHz,1H), 6.42-6.39 (d,J8.4Hz,1H), 4.28 (brs,2H), 2.22 (s,3H)?3CNMR(400MHz, CDC13): 156.52, 141.56, 140.50, 122.99, 107.26, 20.58 IR: 3364, 3199, 2913, 1635, 1601, 1373, 1058, 819 cm4-Amino-2-bromo-3-methyl pyridine (3g) was obtained which was eluted at 25-30% ethyl acetate in hexane.?H NIVIR (300IVIHz, CDC13): oe 7.82-7.80 (d,J5.4Hz,1H), 6.48-6.46 (d,J 5.4Hz,1H), 4.35 (brs,2H), 2.21 (s,3H)?3CNMR(400MHz, CDC13): 152.70, 146.94, 145.05, 116.88, 109.25, 15.73
With the rapid development of chemical substances, we look forward to future research findings about 19230-57-0.
Reference:
Patent; GLENMARK PHARMACEUTICALS LIMITED; BHIRUD, Shekhar Bhaskar; KADAM, Suresh Mahadev; KANSAGRA, Bipin Parsottam; BHADANE, Shailendra Nilkanth; KALE, Shrikrishna Kantilal; PATIL, Ulhas Digambar; (57 pag.)WO2017/56031; (2017); A1;,
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