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Method for preparing 3-methyl-4-aminobenzoic acid through catalytic hydrogenation

An aminobenzoic acid, catalytic hydrogenation technology, applied in chemical instruments and methods, preparation of cyanide reaction, preparation of organic compounds, etc., can solve the problems of many by-products, complicated operation and high cost

Inactive Publication Date: 2017-12-22
中涛新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of catalytic hydrogenation to prepare 3- Methyl-4-aminobenzoic acid method

Method used

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  • Method for preparing 3-methyl-4-aminobenzoic acid through catalytic hydrogenation
  • Method for preparing 3-methyl-4-aminobenzoic acid through catalytic hydrogenation
  • Method for preparing 3-methyl-4-aminobenzoic acid through catalytic hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 1000ml beaker, add 36.2 grams (0.2mol) of 3-methyl-4-nitrobenzoic acid and 300ml of water, and adjust the pH with 25% sodium hydroxide under stirring until the reaction solution is alkaline;

[0029] Then the above solution is poured into a 1L autoclave, 3.0 g of Raney nickel catalyst is added, the autoclave is covered with a locking bolt, the stirring is started, nitrogen is charged into the autoclave to a pressure of 2.0 MPa in the autoclave, and the nitrogen inlet valve is closed. After 30 minutes, the pressure in the autoclave does not decrease, which proves that the autoclave is well sealed. Replace it with nitrogen and hydrogen three times respectively, fill it with ammonia for 2 minutes, and then pressurize it with hydrogen to 3.50MPa. Under the reaction for about 5h, until the hydrogen pressure no longer drops as the end point of the reaction, the reaction solution is obtained;

[0030] Cool to room temperature after reaction finishes, filter out catalyzer,...

Embodiment 2

[0034] In a 1000ml beaker, add 36.2 grams (0.2mol) of 3-methyl-4-nitrobenzoic acid and 300ml of water, and adjust the pH with 25% aqueous sodium carbonate solution under stirring until the reaction solution is alkaline;

[0035] Then the above solution is poured into a 1L autoclave, 2.0g of Raney nickel catalyst is added, the autoclave is covered with a locking bolt, the stirring is started, nitrogen is charged into the autoclave to a pressure of 2.0MPa in the autoclave, and the nitrogen inlet valve is closed. After 30 minutes, the pressure in the autoclave does not drop, which proves that the autoclave is well sealed. Replace it with nitrogen and hydrogen three times respectively, fill it with ammonia for 2 minutes, and then pressurize it with hydrogen to 4.50MPa. Under the reaction for about 1h, until the hydrogen pressure does not drop as the end point, the reaction solution is obtained;

[0036] Cool to room temperature after reaction finishes, filter out catalyzer, filtra...

Embodiment 3

[0039] In a 1000ml beaker, add 36.2 grams (0.2mol) of 3-methyl-4-nitrobenzoic acid and 300ml of water, and adjust the pH with 25% sodium hydroxide under stirring until the reaction solution is alkaline and clear;

[0040]Then the above solution is poured into a 1L autoclave, 1.5 g of Raney nickel catalyst is added, the autoclave is covered with a locking bolt, the stirring is started, nitrogen is charged into the autoclave to a pressure of 2.0 MPa in the autoclave, and the nitrogen inlet valve is closed. After 30 minutes, the pressure in the autoclave does not decrease, which proves that the autoclave is well sealed. Replace it with nitrogen and hydrogen three times respectively, fill it with ammonia for 2 minutes, and then pressurize it with hydrogen to 3.50MPa. The reaction was carried out for about 8 hours until the hydrogen pressure did not drop as the end point, and the reaction solution was obtained;

[0041] Cool to room temperature 5-30 ℃ after reaction finishes, filte...

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Abstract

The invention provides a method for preparing 3-methyl-4-aminobenzoic acid through catalytic hydrogenation, belonging to the technical field of chemical synthesis. The method comprises the following steps: adding 3-methyl-4-nitrobenzoic acid and a solvent into a reaction vessel so as to obtain a 3-methyl-4-nitrobenzoic acid solution, and adjusting the pH value of the solution to be alkaline; pouring the obtained alkaline aqueous solution into an autoclave, adding a catalyst, respectively carrying out replacement with nitrogen and hydrogen for three times, introducing ammonia gas for 2 minutes, carrying out pressurizing with hydrogen to 3.45 MPa to 4.50 MPa, and carrying out a reaction under the pressure of 4.50 to 2.50 MPa at 100 to 160 DEG C so as to obtain a reaction solution; and subjecting the reaction solution to post-processing so as to obtain the 3-methyl-4-aminobenzoic acid. The method provided by the invention has the advantages of easily-available raw materials, simple operation, low production amount of three wastes, environmental friendliness, capability of reaching a mole yield up to 90%, and more applicability to industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing 3-methyl-4-aminobenzoic acid by catalytic hydrogenation. technical background [0002] 3-Methyl-4-aminobenzoic acid is an important intermediate in the synthesis of dyes and medicines, and is mainly used in the synthesis of Telmisartan in the pharmaceutical industry. Telmisartan is an angiotensin (AT) Ⅱ receptor antagonist with the longest half-life, and is the antihypertensive drug with the longest antihypertensive effect of sartan. Due to the long-term dependence of hypertensive patients on drugs, this product is the only drug among angiotensin Ⅱ receptor antagonists that only needs to be taken once a day, and the incidence of side effects is significantly lower than that of similar drugs. At the same time, with the aging trend of the global population, there is a greater need for effective and safe antihypertensive drugs AT II ant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/04C07C229/60
CPCC07C227/04C07C229/60
Inventor 蔡治国王佳旭田蕾孙豪健刘晓黎孙倩
Owner 中涛新材料有限公司
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