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Preparation method of aminomethylbenzoic acid

A technology of aminotoluic acid and aminomethylbenzoic acid, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, etc., can solve the problems of many by-products, complicated preparation process, and low product yield. Achieve the effects of less by-products, simple production process and high product yield

Inactive Publication Date: 2018-11-30
周道平
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation method of the most commonly used aminotoluic acid in industry is: take 4-chloromethylbenzoic acid as raw material, add ammonium carbonate as catalyst, obtain product through ammonification, acidification, removal of impurities and ammonia water neutralization, due to the need to add Catalyst, resulting in many by-products, complex preparation process, and low product yield

Method used

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  • Preparation method of aminomethylbenzoic acid
  • Preparation method of aminomethylbenzoic acid
  • Preparation method of aminomethylbenzoic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0026] A kind of preparation method of aminotoluic acid in the embodiment of the present invention comprises:

[0027] The 4-chloromethylbenzoic acid that takes 40g is dissolved in the methanol of 1100g, obtains mixed solution;

[0028] Add 70g of strong ammonia water (mass fraction is 25%) in mixed solution, control temperature is 60 ℃, and working pressure is 0.3Mpa, carries out reaction 4h in titanium material reaction container, makes 4-chloromethylbenzoic acid change into 4 -aminomethylbenzoic acid, obtain aminomethylbenzoic acid after vacuum filtration, figure 1 It is the high-performance liquid chromatogram (HPLC) of the aminotoluic acid gained in Example 1, as can be seen from the figure, the purity of aminotoluic acid in the resulting product reaches 99.51%, and the retention time is 4.94min. Sample analysis unit: Hunan Dongting Pharmaceutical Industry limited company.

[0029] Chemical reaction process of the present invention is:

[0030]

Embodiment 2

[0032] A kind of preparation method of aminotoluic acid in the embodiment of the present invention comprises:

[0033] The 4-chloromethylbenzoic acid that takes 50g is dissolved in the methanol of 900g, obtains mixed solution;

[0034] Add 80g of concentrated ammonia water (mass fraction is 28%) in mixed solution, control temperature is 80 ℃, and working pressure is 0.5Mpa, carries out reaction 1h in titanium material reaction vessel, makes 4-chloromethylbenzoic acid change into 4 -aminomethylbenzoic acid, obtain aminomethylbenzoic acid after vacuum filtration, figure 2 It is the high-performance liquid chromatogram (HPLC) of the aminotoluic acid obtained in Example 2, as can be seen from the figure, the purity of aminotoluic acid in the resulting product reaches 99.55%, and the retention time is 4.93min. Sample analysis unit: Hunan Dongting Pharmaceutical Industry limited company.

Embodiment 3

[0036] A kind of preparation method of aminotoluic acid in the embodiment of the present invention comprises:

[0037] The 4-chloromethylbenzoic acid that takes 35g is dissolved in the methanol of 1300g, obtains mixed solution;

[0038] Add the strong ammoniacal liquor (massfraction is 26%) of 60g in mixed solution, control temperature is 40 ℃, and working pressure is 0.2Mpa, carries out reaction 5h in glass-lined reaction vessel, makes 4-chloromethylbenzoic acid change into 4 -aminomethylbenzoic acid, obtain aminomethylbenzoic acid after vacuum filtration, image 3 It is the high-performance liquid chromatogram (HPLC) of embodiment 3 gained aminotoluic acid, as can be seen from the figure, the purity of aminotoluic acid in the obtained product reaches 99.55%, and retention time is 4.95min, sample analysis unit: Hunan Dongting Pharmaceutical Industry limited company.

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Abstract

The invention discloses a preparation method of aminomethylbenzoic acid, which belongs to the technical field of drug synthesis. The preparation method comprises the following steps: dissolving 4-chloromethyl-benzoic acid in methanol, and obtaining a mixed solution; and adding a concentrated ammonia water into the mixed solution, controlling the temperature at 40 to 80 DEG C, reacting in a reaction container, enabling the 4-chloromethyl-benzoic acid to be converted to 4-aminomethylbenzoic acid, performing the solid-liquid separation, and obtaining aminomethylbenzoic acid. According to the preparation method of the aminomethylbenzoic acid, the methanol is used as the solvent, the 4-aminomethylbenzoic acid with high purity can be prepared without adding a catalyst, fewer byproducts are produced in the reaction process, and the product yield is relatively high; the consumption of the ammonia water is greatly reduced, the recovery cost of the ammonium water is reduced, and the environmental pollution caused by the ammonium can be reduced; and the requirement for equipment is not high, the cost is relatively low, the production process is simple, and mass popularization can be realized.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a preparation method of aminomethylbenzoic acid. Background technique [0002] The chemical name of aminomethylbenzoic acid is 4-aminomethylbenzoic acid (Aminomethylbenzoic Acid), and the molecular formula is C 8 h 9 NO 2 , with a molecular weight of 151.16. Aminomethylbenzoic acid is both a drug and a pharmaceutical intermediate. It is a powerful hemostatic drug with anti-fibrinolytic hemostatic effect. It has remarkable hemostatic effect, mild side effects, and high drug safety. It is suitable for many The treatment of various types of bleeding symptoms; at the same time, it is also a key intermediate for the preparation of another hemostatic drug - tranexamic acid, which has a large market demand and is a high value-added product. At present, the preparation method of the most commonly used aminotoluic acid in industry is: take 4-chloromethylbenzoic a...

Claims

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Application Information

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IPC IPC(8): C07C227/06C07C229/38
CPCC07C227/06C07C229/38
Inventor 周道平
Owner 周道平
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