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Method for preparing 3-aminophthalic acid hydrochloride

A technology of aminophthalic acid hydrochloride and nitrophthalic acid, applied in the preparation of organic compounds, chemical instruments and methods, preparation of cyanide reactions, etc. Diformic acid is unstable in nature, difficult to store, etc., to achieve the effect of low cost, low equipment requirements, and easy control

Inactive Publication Date: 2015-12-30
ENANTIOTECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the above-mentioned technical problems, the invention provides a kind of method for preparing 3-aminophthalate hydrochloride dihydrate, because it exists with the form of hydrochloride complex, when reacting, can not to Its own chemical properties have an impact, and at the same time, it solves the problem that 3-aminophthalic acid itself is unstable, perishable, and difficult to store

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 500g of mixed solvent of ethanol and dimethyl sulfoxide (mass ratio 1:1) into a 2L autoclave, then add 50g of 3-nitrophthalic acid until completely dissolved in the solvent, stir evenly; replace with nitrogen The air in the kettle was cooled to 5°C after 3 times, and nitrogen gas was continued to be introduced, and 0.14 g of platinum black was added under the protection of nitrogen gas; after 3 times of replacement with hydrogen gas, hydrogen gas was continued to be charged until the pressure in the reaction vessel was 0.14 MPa, and the hydrogenation reaction was carried out. After the hydrogenation reaction is finished, remove the catalyst by filtration and take the filtrate; cool the obtained filtrate to 0°C, add 58.4 g of concentrated hydrochloric acid with a concentration of 12mol / L dropwise to carry out the complexation reaction, stir, and continue stirring at this temperature after the dropwise addition is completed 2 hours; the product after the complexation r...

Embodiment 2

[0026] Add a mixed solvent of 600g tetrahydrofuran and toluene (mass ratio 1:1) into a 2L high-pressure reactor, then add 50g of 3-nitrophthalic acid until it is completely dissolved in the solvent, and stir evenly; replace the air in the reactor with nitrogen After 3 times, cool down to 10°C, continue to feed nitrogen, and add 0.18 g of palladium black under the protection of nitrogen; after 3 replacements with hydrogen, continue to fill hydrogen until the pressure in the reaction vessel is 0.2 MPa, and carry out hydrogenation reaction. , remove catalyst by filtration, get filtrate; Gained filtrate is cooled to 0 ℃, dropwise concentration is the concentrated hydrochloric acid 25.6g of 12mol / L to carry out complexation reaction, stir, after dropwise addition, continue stirring at this temperature for 2 hours; The product after the complexation reaction was centrifuged, and the resulting solid was dried in a double-cone vacuum dryer at 30°C for 4 hours to obtain 3-aminophthalate...

Embodiment 3

[0028] Add 750g of solvent in a 2L autoclave, and the solvent is mixed uniformly with acetonitrile, acetone, pentane, n-hexane, n-heptane, and tert-butyl methyl ether with a mass ratio of 1:1:1:1:1:1 Then add 50g of 3-nitrophthalic acid to completely dissolve in the solvent, stir evenly; replace the air in the reactor with nitrogen for 3 times, then cool down to 0°C, continue to feed nitrogen, and add platinum black under the protection of nitrogen 0.05g; after 3 times of replacement with hydrogen, continue to fill the reaction vessel with hydrogen until the pressure in the reaction vessel is 0.2MPa, and carry out the hydrogenation reaction. 186.1g of 12mol / L concentrated hydrochloric acid was used for the complexation reaction, stirred, and after the dropwise addition was completed, the stirring was continued at this temperature for 2 hours; the product after the complexation reaction was centrifuged, and the obtained solid was placed in a double-cone vacuum dryer at 35°C It ...

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Abstract

The invention discloses a method for preparing 3-aminophthalic acid hydrochloride. The method comprises the following synthesis steps of (1) dissolution; (2) nitrogen displacement; (3) hydrogenation reaction; (4) complexation reaction; (5) centrifugal drying. According to the method, the 3-aminophthalic acid hydrochloride is directly synthesized from a raw material 3-nitrophthalic acid by combined treatment procedures of dissolution, nitrogen displacement, hydrogenation reaction, complexation reaction and centrifugal drying, and the 3-nitrophthalic acid is converted into a complex form of the 3-aminophthalic acid hydrochloride, so that the problems of instability, high deterioration rate, purity reduction caused by short-time storage and harm to storage and long-distance transportation of the 3-nitrophthalic acid are solved; in addition, the method has the advantages of convenience in operation, easiness in control, low requirements on equipment, short flow, lower cost, high product purity and high yield, and is adapted to industrial production.

Description

technical field [0001] The invention relates to a method for preparing 3-aminophthalate hydrochloride dihydrate, in particular to a method for directly synthesizing 3-aminophthalate with 3-nitrophthalic acid as raw material salt dihydrate method. Background technique [0002] 3-aminophthalic acid is an important organic synthesis intermediate, which is widely used in medicine, dyes, etc., but because 3-aminophthalic acid is unstable and easy to deteriorate, even short-term storage will cause The purity is reduced, which is not conducive to storage and long-distance transportation, etc., and further improvement is needed. [0003] At present, there are few literature reports on the method for preparing 3-aminophthalic acid. In Chinese patent CN201510021669.3, a method for preparing 3-aminophthalic acid is provided, using 3-nitrophthalic acid as The raw material is prepared through high-pressure hydrogenation under the action of a catalyst; Chinese patent CN200710020080.7 di...

Claims

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Application Information

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IPC IPC(8): C07C229/62C07C227/04
Inventor 徐亮黄志鸿李彦雄甄伟达高蕊谭格良
Owner ENANTIOTECH CORP
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