A method for the synthesis of amides from heterocyclic compounds catalyzed by non-metallic porous carbon
A technology for amide compounds and heterocyclic compounds is applied in the synthesis of amide compounds from non-metal porous carbon catalyzed heterocyclic compounds and the synthesis of amide derivatives, which can solve the problems of lack of catalyst systems and no major breakthroughs. Achieve the effect of low cost, short route and easy availability of raw materials
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Embodiment 1、2
[0021] Embodiment 1, the synthesis of 2-pyridinecarboxamide
[0022] (1) Preparation of porous carbon material: 6 g of fructose was dissolved in 50 g of distilled water, then 4 g of fumed silica was added, and stirred at 25°C for 12 hours. The resulting mixture was placed at 40 o C was dried for 48 hours, then carbonized at 600°C for 6 hours under inert atmosphere to obtain black powder; the black powder was treated with a template removing agent for 12 hours, filtered, washed with distilled water until the pH was about 7, and then vacuum-dried to obtain a porous carbon material ;
[0023] (2) Preparation of 2-pyridinecarboxamide: Weigh 0.1 g of porous carbon material, 0.5 g of 2-picoline, and 0.5 g of ammonia water, put them into the autoclave, and after 3 times of replacement with oxygen, add oxygen to 0.1 MPa, The temperature was raised to 200°C, and the reaction was carried out for 0.5 hour; after the reaction was completed, it was cooled to room temperature; the reactio...
Embodiment 2、4
[0025] Embodiment 2, the synthesis of 4-pyridinecarboxamide
[0026] (1) Preparation of nitrogen atom-doped porous carbon materials: 6 g of glucose, 15 g of silica sol, and 5 g of urea were dissolved in 50 g of distilled water, and stirred at 100 °C for 36 hours. The resulting mixture was dried at 150°C for 2 hours, and then carbonized at 1200°C for 2 hours under an inert atmosphere to obtain a black powder. The black powder was treated with a template removing agent for 12 hours, filtered, washed with distilled water until the pH was about 7, and then vacuum-dried to obtain a nitrogen-doped porous carbon material.
[0027] (2) Synthesis of 4-pyridinecarboxamide: Weigh 0.1 g of nitrogen-doped porous carbon material, 0.5 g of 4-picoline, and 0.4 g of urea, put them in the autoclave, and after 3 times of replacement by oxygen, the solution is filled with oxygen. to 10 MPa, heated to 50 °C, and reacted for 48 hours; after the reaction was completed, cooled to room temperature. ...
Embodiment 3、3
[0028] Embodiment 3, the synthesis of 3-pyridinecarboxamide
[0029] (1) Preparation of sulfur atom-doped porous carbon material: Dissolve 6 g of sucrose, 4 g of fumed silica, and 2 g of concentrated sulfuric acid in 50 g of distilled water, and stir at room temperature for 12 hours to obtain a homogeneous mixture. Then, the obtained mixture was dried at 120°C for 12 hours, and then carbonized at 900°C for 4 hours to obtain black powder; the black powder was treated with a template removing agent for 12 hours, filtered, washed with distilled water until the pH was about 7, and then vacuum-dried to obtain Sulfur-doped porous carbon materials.
[0030] (2) Synthesis of 3-pyridinecarboxamide: Weigh 0.1 g of nitrogen-doped porous carbon material, 1.0 g of 3-picoline, and 1.0 g of ammonium nitrate, put them into an autoclave, and after 3 times of replacement with oxygen, the solution is charged. Oxygen to 5 MPa, the temperature was raised to 120 °C, and the reaction was carried ou...
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