Preparation of 4-pyridinecarboxamide_industrial additives

Preparation background and overview of 4-pyridinecarboxamide

4-Pyridinecarboxamide is a pyridine derivative containing an amide functional group. Polycarbonate amide functional group is a very important type of functional group in organic compounds. Many natural compounds, pharmaceutical intermediates and high value-added fine chemicals contain amide functional groups.

Preparation of 4-pyridinecarboxamide

Preparation Report 1 of 4-pyridinecarboxamide,

(1) Preparation of nitrogen atom-doped porous carbon materials: Dissolve 6 g glucose, 15 g silica sol, and 5 g urea in 50 g distilled water, and stir at 100°C for 36 hours. The obtained mixture was dried at 150°C for 2 hours, and then carbonized at 1200°C for 2 hours under inert atmosphere conditions to obtain black powder. The black powder is treated with a template removal agent for 12 hours, filtered, washed with distilled water until the pH is about 7, and then dried in a vacuum to obtain a nitrogen-doped porous carbon material.

(2) Synthesis of 4-pyridinecarboxamide: Weigh 0.1g nitrogen-doped porous carbon material, 0.5g 4-methylpyridine, and 0.4g urea, add them to the high-pressure reaction kettle, and replace them with oxygen three times. , fill with oxygen to 10 MPa, raise the temperature to 50°C, and react for 48 hours; after the reaction is completed, cool to room temperature. The reaction solution was analyzed by gas chromatography, and the yield of 4-pyridinecarboxamide was 81%.

Preparation Report 2 of 4-Pyridinecarboxamide

Add 100mg ferric oxide, 100mg tricobalt tetroxide and 10 battery grade lithium carbonate to 6g tert-amyl alcohol, 0mg manganese dioxide (mass percentage in the mixture: 4.6%), 60mg 4-cyanopyridine (in the mixture Mass percentage: 0.91%), 200uL water (mass percentage in the mixture: 3.0%), mix evenly; react at 80°C for 24 hours, 4-cyanopyridine conversion rate is 99.0%, corresponding selection of 4-pyridinecarboxamide Safety is 99.0%.

References

[1] [Chinese invention] CN202010203137.2 A method for synthesizing amide compounds from heterocyclic compounds using non-metal porous carbon catalysis

[2] [Chinese invention] CN201910531204.0 Method for preparing amide compounds by using oxide materials to catalyze the hydration of organic nitriles