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Synthesis method of piperidine carboxylic acid amide drug intermediate N-(2,6-dimethyl benzene)-4-pyridine carboxamide
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Paragraph 0015; 0016, (2016/11/09)
A synthesis method of piperidine carboxylic acid amide drug intermediate N-(2,6-dimethyl benzene)-4-pyridine carboxamide comprises steps as follows: 1.1 mol of pyridine-4-formamide and 600-620 ml of nitromethane are added to a reaction container provided with a stirrer and a thermometer, the stirring speed is controlled to range from 130 rpm to 160 rpm, 0.4-0.42 mol of cuprous bromide is added in batches, the temperature of the solution is increased to 100-105 DEG C, the solution reacts for 2-3 h, filtration is performed, a filtrate is added to the reaction container again, 1.1-1.3 mol of 2,6-xylidine is added dropwise, the stirring speed is kept for 5-6 h after addition, the temperature of the solution is decreased to 15-18 DEG C, solids separate out, filtration is performed, the solids are washed with ethyl acetate, N-(2,6-dimethyl benzene)-4-pyridine carboxamide bromate is obtained and dissolved in 1,100 ml of a potassium nitrate solution, decolorization is performed with a molecular sieve, a sodium sulfite solution is added to adjust the pH to range from 9 to 10, the temperature of the solution is decreased to 3-5 DEG C, solids separate out, filtration is performed, the solids are washed with a salt solution, dehydrated with a dehydrating agent and recrystallized in chlorobenzene, and the N-(2,6-dimethyl benzene)-4-pyridine carboxamide is obtained.