1351413-50-7Relevant articles and documents
Method for synthesizing 1-methyl-2-oxo-1, 2-dihydropyridine-4-base boric acid
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Paragraph 0015; 0016; 0017, (2017/09/01)
The invention discloses a method for synthesizing 1-methyl-2-oxo-1, 2-dihydropyridine-4-base boric acid. The method includes (1), adding sodium hydride and methyl iodide into 2-hydroxyl-4-bromopyridine and N-N-dimethylformamide and carrying out reaction to obtain intermediate crude products; (2), dissolving the intermediate crude products obtained at the step (1) into first dioxane, sequentially adding potassium acetate, borate and catalysts into the first dioxane, carrying out heating reflux for 12-15 h and completely carrying out reaction; (3), dissolving second products obtained at the step (2) in second dioxane and hydrochloric acid, stirring the second products, the second dioxane and the hydrochloric acid at the temperatures of 25 DEG C for 12 hours, completely carrying out reaction, carrying out extraction and drying solvents by distillation to obtain the clean 1-methyl-2-oxo-1, 2-dihydropyridine-4-base boric acid. The 2-hydroxyl-4-bromopyridine is used as a raw material, and the N-N-dimethylformamide is used as a solvent. The volume of the first dioxane is five times the volumes of the intermediate crude products. The method has the advantages that intermediates do not need to be purified owing to designed synthesis routes, only final products need to be purified, the total yield of the three steps ranges from 40% to 60%, raw materials for the 1-methyl-2-oxo-1, 2-dihydropyridine-4-base boric acid are inexpensive, experiments are convenient to operate, and mass production can be hopefully implemented.