Co-crystal product of 2-aminobenzamide and oxalic acid and preparation method assisted by microwave irradiation
An aminobenzamide and microwave irradiation technology, which is applied in the preparation of carboxylic acid amides, carboxylate salts, and carboxylate salts, can solve the problems of coalescence, impure crystal products, uneven product particle size distribution, etc. Enhanced dispersibility, enhanced solubility, and improved crystal morphology
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Embodiment 1
[0030] The microwave radiation-assisted preparation method of the eutectic product of 2-aminobenzamide and oxalic acid comprises the following steps:
[0031] (1) Under the condition that the stirring rate is 200rpm and the temperature is 10°C, 1g of 2-aminobenzamide is added to a microwave reactor filled with 10g of methanol solvent, stirred at a constant temperature for 10min until the dissolution is complete, and a dissolved solution is obtained. , the massfraction of 2-aminobenzamide in the dissolving solution is 10%;
[0032] (2) Continue to add 1 g of oxalic acid into the microwave reactor at 10°C, and stir at a constant temperature until it dissolves completely and becomes a clear solution;
[0033] (3) Under the condition of 10°C, set the microwave radiation power in the microwave reactor to 100W, turn on the microwave radiation reaction for 2 hours, and obtain the crystal slurry;
[0034] (4) Suction filter and wash the crystal slurry to obtain a filter cake, and dry...
Embodiment 2
[0037] The microwave radiation-assisted preparation method of the eutectic product of 2-aminobenzamide and oxalic acid comprises the following steps:
[0038] (1) Under the condition that the stirring rate is 300rpm and the temperature is 20°C, 2g of 2-aminobenzamide is added to a microwave reactor filled with 10g of dimethylformamide solvent, and stirred at constant temperature for 20min until it dissolves completely to obtain Dissolving solution, at this moment, the massfraction of 2-aminobenzamide in the dissolving solution is 20%;
[0039] (2) Continue to add 2 g of oxalic acid into the microwave reactor at 20°C, and stir at a constant temperature until the solution is completely dissolved and becomes a clear solution;
[0040] (3) Under the condition of 20°C, set the microwave radiation power in the microwave reactor to 200W, and turn on the microwave reaction for 3 hours to obtain the crystal slurry;
[0041] (4) Suction filter and wash the crystal slurry to obtain a fi...
Embodiment 3
[0044] The microwave radiation-assisted preparation method of the eutectic product of 2-aminobenzamide and oxalic acid comprises the following steps:
[0045] (1) Under the condition that the stirring rate is 300rpm and the temperature is 30°C, 3g of 2-aminobenzamide is added into a microwave reactor filled with 10g of methyl ethyl ketone solvent, stirred at a constant temperature for 30min until it dissolves completely, to obtain Dissolving solution, at this moment, the massfraction of 2-aminobenzamide in the dissolving solution is 30%;
[0046] (2) Continue to add 3g of oxalic acid into the microwave reactor at 30°C, and stir at constant temperature until the solution is completely dissolved and becomes a clear solution;
[0047] (3) Under the condition of 30°C, set the microwave radiation power in the microwave reactor to 300W, and turn on the microwave reaction for 4 hours to obtain the crystal slurry;
[0048] (4) Suction filter and wash the crystal slurry to obtain a filt...
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