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Process for continuously producing an aminobenzoate derivative, and synthesis system thereof

A technology of aminobenzoate and nitrobenzoic acid, which is applied in the field of continuous production of aminobenzoate derivatives and its synthesis system, which can solve the problems of unstable product quality, high labor intensity, and high labor cost , to achieve the effects of low conversion rate of esterification reaction, high production efficiency and low labor intensity

Active Publication Date: 2020-01-03
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although iron powder reduction has low cost, safe reaction, and low technical requirements for workers, the iron sludge produced is solid hazardous waste, and there are still problems such as a large amount of wastewater. It has been listed as a backward and eliminated process, and new projects have banned the use of it Technology, the technology already in production is also required to be phased out within a time limit
[0004] At present, the catalytic hydrogenation technology in the field of fine chemical industry is basically a batch production technology, and most of the hazards come from the operation of workers.
At the same time, intermittent production also brings disadvantages such as unstable product quality, high labor intensity, and high labor costs.

Method used

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  • Process for continuously producing an aminobenzoate derivative, and synthesis system thereof
  • Process for continuously producing an aminobenzoate derivative, and synthesis system thereof
  • Process for continuously producing an aminobenzoate derivative, and synthesis system thereof

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Embodiment 1

[0048] Reaction raw materials: ethanol (commercially available industrial ethanol, content 99%); p-nitrobenzoic acid (commercially available, content 98%); hydrogen (commercially available, content 99%).

[0049] Esterification catalyst: industrial concentrated sulfuric acid (commercially available, content 98%) or p-toluenesulfonic acid (commercially available, content 99%);

[0050] Catalytic hydrogenation reaction catalyst: commercially available palladium carbon containing 1-5% palladium; dosage is 0.5%-1% of p-nitrobenzoic acid.

[0051] Solvent: the solvent of esterification reaction and catalytic hydrogenation reaction is ethanol (commercially available industrial ethanol, content 99%);

[0052] Put 1380Kg of ethanol into the esterification reactor 12, 100Kg of p-nitrobenzoic acid, 20Kg of concentrated sulfuric acid, open the circulation pump 24 of the esterification reactor 12, heat up to 75°C, and keep warm for 1 hour after the cycle residence time, then go to the est...

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PUM

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Abstract

The invention provides a process for continuously producing an aminobenzoate derivative, and a synthesis system thereof. The process comprises: putting a nitrobenzoic acid derivative, ethanol and a first catalyst into an esterification reaction device, and reacting for 1-1.5 h at a temperature of 70-75 DEG C; supplementing a nitrobenzoic acid derivatives, ethanol and a first catalyst into the esterification reaction device; making the liquid in the esterification reaction device flow into a dehydration esterification kettle; heating to azeotrope the ethanol-water in the dehydration esterification kettle, evaporating the azeotrope out of the dehydration esterification kettle, collecting the azeotrope, and discharging the liquid in the dehydration esterification kettle into a middle liquid storage groove; and making the liquid in the middle liquid storage groove flow into a hydrogenation reaction device, and carrying out a hydrogenation reaction under the action of a second catalyst at areaction temperature of 100-120 DEG C to obtain the product, wherein the pressure is kept at 0.6-1 Mpa. According to the invention, the process has advantages of continuous production and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a process for continuously producing aminobenzoate derivatives and a synthesis system thereof. Background technique [0002] Aminobenzoate derivatives are important intermediates in the synthesis of various drugs. This type of drug can locally and reversibly block the occurrence of sensory nerve impulses at the site of administration. Typical representative drugs are: benzocaine, procaine hydrochloride, tetracaine hydrochloride, procainamide hydrochloride, etc. [0003] The industrial production of aminobenzoic acid ester derivatives is basically obtained by esterification of nitrobenzoic acid with alcohol and then reduction. The esterification reaction is a reversible reaction, and the yield cannot be very high. Intermittent production requires a lot of technical operations for workers, which is likely to cause problems such as unstable quality and large consumption...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/04C07C229/60B01J19/18B01J4/00C07C201/12C07C205/58C07C205/57
CPCC07C227/04C07C201/12B01J19/18B01J4/007B01J2219/00094C07C229/60C07C205/58C07C205/57
Inventor 贾建洪余国义沙洋澄张久明冯东李益珠佘远斌
Owner ZHEJIANG UNIV OF TECH
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