Synthesis method of pharmaceutical intermediate m-aminobenzoic acid

The technology of an aminobenzoic acid and a synthesis method is applied in the field of synthesis of a pharmaceutical intermediate m-aminobenzoic acid, and can solve the problems of complicated process and low final yield, and achieves reduction of intermediate links, shortening of reaction time, and improvement of reaction yield. Effect

Inactive Publication Date: 2018-08-17
CHENGDU ZHONGHENG HUATIE TECH CO LTD
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Problems solved by technology

[0002] M-aminobenzoic acid is mainly used in the synthesis of pharmaceutical intermediates, but most of the existing synthetic methods use iron powder as a reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method method, which has important economic significance for further improving the quality and yield of products and reducing the content of by-products

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  • Synthesis method of pharmaceutical intermediate m-aminobenzoic acid

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example 1

[0011] Add 3 mol of cuprous chloride, 4 mol of toluene solution, and 5 mol of m-nitrobenzoic acid solution in the reaction vessel, raise the temperature of the solution to 60°C, control the stirring speed at 110rpm, keep it for 90min, and oxidize it with 10% mass fraction of hydrogen Adjust the pH of the solution to 9 with sodium solution, reduce the temperature of the solution to 5°C, and precipitate crystals, add 6L mass fraction of 30% ethanol solution for washing, mass fraction of 40% sodium chloride solution for washing, mass fraction of 50% nitromethane solution for washing , the mass fraction is 60% ethylenediamine solution washing, dehydrating with anhydrous sodium sulfate dehydrating agent, obtains 357.57g of finished m-aminobenzoic acid, yield 87%.

example 2

[0013] Add 3 mol of cuprous chloride, 4.5 mol of toluene solution, and 5 mol of m-nitrobenzoic acid solution in the reaction vessel, raise the temperature of the solution to 65°C, control the stirring speed at 120rpm, keep it for 100min, and use a mass fraction of 12% hydrogen Adjust the pH of the solution to 9.5 with sodium oxide solution, reduce the temperature of the solution to 7°C, and precipitate crystals, add 6L of 32% ethanol solution for washing, 42% of sodium chloride solution for washing, and 53% of nitromethane solution for washing Washing, washing with ethylenediamine solution with a mass fraction of 63%, and dehydrating with anhydrous magnesium sulfate dehydrating agent to obtain 374.01 g of finished m-aminobenzoic acid with a yield of 91%.

example 3

[0015] Add 3 mol of cuprous chloride, 5 mol of toluene solution, and 5 mol of m-nitrobenzoic acid solution in the reaction vessel, increase the temperature of the solution to 70 ° C, control the stirring speed at 130 rpm, keep it for 110 min, and use a mass fraction of 15% for hydrogen oxidation Adjust the pH of the solution to 10 with sodium solution, reduce the temperature of the solution to 10°C, and precipitate crystals, add 6L mass fraction of 35% ethanol solution for washing, mass fraction of 45% sodium chloride solution for washing, mass fraction of 56% nitromethane solution for washing , the mass fraction is 65% ethylenediamine solution washing, dehydrating with anhydrous sodium sulfate dehydrating agent, obtains 382.23g of finished product m-aminobenzoic acid, yield 93%.

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Abstract

The invention relates to a synthesis method of a pharmaceutical intermediate m-aminobenzoic acid. The synthesis method mainly comprises: adding 3 mol cuprous chloride, 4-5 mol toluene solution and 5 mol m-nitrobenzoic acid solution to a reaction container, heating the solution to a temperature of 60-70 DEG C, controlling the stirring speed at 110-130 rpm, maintain for 90-110 min, adjusting the pHvalue of the solution to 9-10 with a sodium hydroxide solution, cooling the solution to a temperature of 5-10 DEG C, crystallizing, adding 6 L ethanol solution, washing, washing with a sodium chloridesolution, washing with a nitromethane solution, washing with an ethylenediamine solution, and dewatering with a dewatering agent to obtain the finished product m-aminobenzoic acid.

Description

technical field [0001] The invention relates to a method for synthesizing a drug intermediate m-aminobenzoic acid. Background technique [0002] M-aminobenzoic acid is mainly used in the synthesis of pharmaceutical intermediates, but most of the existing synthetic methods use iron powder as a reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method method, which has important economic significance for further improving the quality and yield of products and reducing the content of by-products. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of drug intermediate m-aminobenzoic acid, comprising the steps: [0004] (i) Add 3mol of cuprous chloride, 4-5mol of toluene solution, and 5mol of m-nitrobenzoic acid solution in the reaction vessel, raise the temperature of the solution to 60-70°C, control the stirring speed at 110-130rpm,...

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 彭响亮
Owner CHENGDU ZHONGHENG HUATIE TECH CO LTD
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