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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

Active Publication Date: 2022-05-20
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Zhang Xiaopeng et al [Synthesis of anthranilamide compounds, Progress in Chemistry, 2017, 29(11): 1351-1356] summarized the research progress in the synthesis of anthranilamide compounds, mainly introducing several anthranilamide compounds The synthesis method of amide, for example, using anthranilyl halide as a substrate, organic amine as a nucleophile, directly synthesizes anthranilamide through a nucleophilic substitution reaction, but there are problems in the prepared anthranilamide product , the particle size distribution of the product is uneven, and there is agglomeration phenomenon, which leads to the impurity of the crystal product. Therefore, it is urgent to find a new eutectic ligand to form a eutectic product with 2-aminobenzamide

Method used

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  • Co-crystal product of 2-aminobenzamide and oxalic acid and preparation method assisted by microwave irradiation
  • Co-crystal product of 2-aminobenzamide and oxalic acid and preparation method assisted by microwave irradiation
  • Co-crystal product of 2-aminobenzamide and oxalic acid and preparation method assisted by microwave irradiation

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Experimental program
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Effect test

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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Abstract

The invention discloses a co-crystal product of 2-aminobenzamide and oxalic acid. The X-ray powder diffraction spectrum of the co-crystal product crystal is at diffraction angle 2θ=7.8±0.1, 8.1±0.1, 12.7±0.1, 15.9±0.1 There are characteristic peaks at 0.1, 17.3±0.1, 19.8±0.1, 23.2±0.1, 25.6±0.1, and 29.7±0.1 degrees, and a microwave radiation-assisted preparation method of a co-crystal product of 2-aminobenzamide and oxalic acid is also disclosed . The invention has the beneficial effects of improving the solubility of the 2-aminobenzamide eutectic product, improving its crystal appearance, and increasing its particle size and bulk density.

Description

technical field [0001] The invention relates to the technical field of chemical engineering crystallization. More specifically, the present invention relates to a microwave radiation-assisted preparation method of a co-crystal product of 2-aminobenzamide and oxalic acid. Background technique [0002] 2-aminobenzamide (C 7 h 8 N 2 O, 136.15g / mol, CAS NO:88-68-6), also known as linaminobenzamide, English name 2-Aminobenzamide, usually light brown to gray-brown crystal powder or tablet, odorless, slightly bitter taste , slightly soluble in water, slightly soluble in ethanol, with a melting point of 111-113°C, 2-aminobenzamide is a kind of intermediate used in organic synthesis, used for the synthesis of raw materials, non-selective, effective polysaccharide fluorescent labeling, The currently prepared 2-aminobenzamide has a small particle size of only 150 μm, and its appearance is as follows: figure 1 As shown, the degree of coalescence is large, the bulk density is small,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/30C07C231/12C07C55/06C07C55/07C07C51/41
CPCC07C237/30C07C231/12C07C55/06C07C55/07C07C51/412
Inventor 欧阳金波那兵周利民刘峙嵘熊国宣
Owner EAST CHINA UNIV OF TECH
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