Extracurricular laboratory: Synthetic route of 3-Bromo-1-methyl-5-nitropyridin-2(1H)-one

According to the analysis of related databases, 16098-21-8, the application of this compound in the production field has become more and more popular.

Application of 16098-21-8, 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. 16098-21-8, name is 3-Bromo-1-methyl-5-nitropyridin-2(1H)-one, molecular formula is C6H5BrN2O3, 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.

To a solution containing 0.60 g (2.57 mmol) of 3- bromo-1-methyl-5-nitropyridin-2 (1H)-one in 120 ml of toluene under a nitrogen atmosphere was added 0.64 ml (5.15 mmol) of 2,4-dimethylaniline, 1.61 g (2.57 mmol) of rac- 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (racemic BINAP), 0.37 g (3.85 mol) of sodium t-butoxide and 1.20 g (1.31 mmol) of tris(dibenzylideneacetone)dipalladium (0). The reaction was heated to 95C overnight. The reaction was cooled to room temperature, diluted with ethyl acetate and washed with saturated sodium bicarbonate. The organic phase was dried over magnesium sulfate. Filtration, removal of solvent and purification of the residue via biotage eluting with 60% ethyl acetate/hexanes gave the desired product with some starting aniline. The material was triturated with hexanes and the solids filtered and dried to afford 0.154 g (21.9%) of product. ¹H NMR (CDC13) 5: 2.22 (s, 3H) , 2.35 (s, 3H) , 3.74 (s, 3H) , 6.72 (bs, 1H), 7 .06 – 7.18 (m, 4H), 8. 06 (d, J = 2.8 Hz, 1H)

According to the analysis of related databases, 16098-21-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2005/99688; (2005); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem