Preparation method of p-aminobenzoyl glutamic acid

A technology of aminobenzoyl glutamic acid and p-nitrobenzoic acid, which is applied in the field of preparation of p-aminobenzoyl glutamic acid, can solve the problems of low yield, polluted environment by waste residue, long reaction time and the like, and achieves high yield. The effect of high rate, high process safety and low production cost

Inactive Publication Date: 2020-01-10
SHE COUNTY JINDONG ECONOMIC & TRADE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method not only has low yield and long reaction time, but also has a large amount of waste residue (iron slime) and waste water to pollute the environment, so a kind of preparation method of p-aminobenzoyl glutamic acid is proposed to solve the above problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of p-aminobenzoyl glutamic acid, the concrete steps are as follows:

[0019] (1) Weigh 10 parts of p-nitrobenzoic acid, 15 parts of oxalyl chloride, 10 parts of solvent dichloroethane and 50 parts of DMF, add nitrobenzoic acid, oxalyl chloride, dichloroethane and DMF into the reaction vessel for For the reaction, the reaction vessel was heated to 50°C and continued to heat for 1 hour. During the heating process of the reaction vessel, the reaction vessel was required to be covered, and the inside of the reaction vessel was continuously stirred at a constant speed to ensure that the nitrobenzoic acid The reaction with thionyl chloride is uniform; after the reaction, put the mixed reactant into the distillation container, and slowly heat the distillation container by means of a water bath, so that the temperature of the distillation container is controlled at 80 ° C, and distilled for 2 hours, Distillation by a distillation vessel to reclaim the solve...

Embodiment 2

[0024] A preparation method of p-aminobenzoyl glutamic acid, the concrete steps are as follows:

[0025] (1) Weigh 11 parts of p-nitrobenzoic acid, 16 parts of oxalyl chloride, 11 parts of solvent dichloroethane and 52 parts of DMF, add nitrobenzoic acid, oxalyl chloride, dichloroethane and DMF into the reaction vessel for To react, heat the reaction vessel to 52°C and continue heating for 1.2h. During the heating process of the reaction vessel, the reaction vessel needs to be covered, and the inside of the reaction vessel should be continuously stirred at a constant speed to ensure that the nitrobenzene The reaction of formic acid and thionyl chloride is uniform; after the reaction, put the mixed reactants into the distillation vessel, and slowly heat the distillation vessel by means of a water bath, so that the temperature of the distillation vessel is controlled at 85°C, and distilled for 2.2 h, by distilling in a distillation vessel to reclaim the solvent and remove hydrog...

Embodiment 3

[0030] A preparation method of p-aminobenzoyl glutamic acid, the concrete steps are as follows:

[0031] (1) Weigh 12 parts of p-nitrobenzoic acid, 18 parts of oxalyl chloride, 12 parts of solvent dichloroethane and 55 parts of DMF, add nitrobenzoic acid, oxalyl chloride, dichloroethane and DMF into the reaction vessel for To react, heat the reaction vessel to 55°C and continue heating for 1.5h. During the heating process of the reaction vessel, the reaction vessel needs to be covered, and the interior of the reaction vessel should be continuously stirred at a constant speed to ensure that the nitrobenzene The reaction of formic acid and thionyl chloride is uniform; after the reaction, put the mixed reactant into the distillation vessel, and slowly heat the distillation vessel by means of a water bath, so that the temperature of the distillation vessel is controlled at 90°C, and distilled for 2.5 h, by distilling in a distillation vessel to reclaim the solvent and remove hydro...

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Abstract

The invention discloses a preparation method of p-aminobenzoyl glutamic acid. The preparation method comprises the following specific steps: adding nitrobenzoic acid, oxalyl chloride, dichloroethane and DMF into a reaction container to react to obtain p-nitrobenzoyl chloride; reacting p-nitrobenzoyl chloride with sodium glutamate to obtain p-nitrobenzoyl glutamic acid; and carrying out reduction,separation, acid precipitation, refining and drying unit processes on the obtained p-nitrobenzoylglutamic acid in the presence of a polar solvent and a catalyst to obtain a finished product, wherein in the reduction process, pH value is adjusted to 6-10 with sodium hydroxide, and then hydrogenation and hydrazine hydrate reduction are carried out. The method is mild in reaction, simple and convenient to operate, high in process safety, low in production cost, green and environmentally friendly, the obtained product is high in purity and yield, the catalyst can be repeatedly used, the solvent can be recycled after being distilled and recycled, a small amount of waste liquid can be discharged up to the standard after being subjected to alkali treatment, environmental pollution is small, and therefore the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a pharmaceutical intermediate, in particular to a preparation method of p-aminobenzoyl glutamic acid. Background technique [0002] P-aminobenzoyl glutamic acid is a key intermediate in the synthesis of folic acid. The so-called pharmaceutical intermediates are actually some chemical raw materials or chemical products used in the process of pharmaceutical synthesis. Such chemical products do not require a pharmaceutical production license and can be produced in ordinary chemical factories, as long as they meet certain requirements. Grade, which can be used for the synthesis of medicines. Our country needs more than 2,000 kinds of raw materials and intermediates for chemical industry every year, with a demand of more than 2.5 million tons. After more than 30 years of development, the chemical raw materials and intermediates required for my country's pharmaceutical production Basically, it can be matched, only a small part needs t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C237/36
CPCC07C231/12C07C201/12C07C231/02
Inventor 刘俊成刘东东张帆
Owner SHE COUNTY JINDONG ECONOMIC & TRADE CO LTD
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