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Preparation method of medicine (actarit intermediate) for rheumatic bone disease

A use, zinc modification technology, applied in the field of medicine, can solve the problems of high toxicity of hydrazine hydrate, not conforming to green chemical industry, difficult to handle, etc., and achieve the effect of improving catalytic activity, improving catalyst reactivity and reducing dosage

Active Publication Date: 2018-10-23
ZIBO VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The synthetic method of this compound that prior art reports at present mainly contains two kinds, and a class is to adopt the method for chemical reduction, as in CN 106083631 A, ferric chloride is used as catalyst, and hydrazine hydrate is used as reducing agent to p-nitrophenylacetic acid Reduction, but the toxicity of hydrazine hydrate is relatively large; Nie Lijuan et al. (Chinese Journal of Pharmaceutical Industry, 2008, Volume 39, No. 12, page 894, the synthesis of Actarit) adopts ammonium sulfide as reducing agent, but the co-production side effects The product sulfur-containing elemental aqueous solution is difficult to handle, does not meet the requirements of green chemical industry; Reduction is carried out in the Fe / AcOH system, but it also produces a large amount of iron-containing wastewater that is difficult to treat

Method used

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  • Preparation method of medicine (actarit intermediate) for rheumatic bone disease
  • Preparation method of medicine (actarit intermediate) for rheumatic bone disease
  • Preparation method of medicine (actarit intermediate) for rheumatic bone disease

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of silicon carbide-supported zinc-modified Pd catalyst:

[0029] Nano silicon carbide 10.0g, PdCl 2 (2.5g, 14.1mmol) and ZnCl 2 (0.32g, 2.35mmol) in 100ml of ethanol / water mixed solution (volume ratio 1:1) and ultrasonically mixed for more than 12h, then use sodium carbonate aqueous solution to adjust the pH of the system to 8-9, dropwise add sodium borohydride water to disperse solution (100ml containing 80mmol of sodium borohydride) for reduction, continued stirring for 6-8h after the dropwise addition, then filtered and washed with water until there was no chloride ion in the filtrate, and vacuum-dried at 40°C to obtain a zinc-modified Pd catalyst supported on silicon carbide.

Embodiment 2

[0031] Nano silicon carbide 10.0g, PdCl 2 (3.5g, 19.7mmol) and ZnCl 2 (0.34g, 2.46mmol) was ultrasonically mixed in 100ml of ethanol / water mixed solution (1:1 volume ratio) for more than 12h, then adjusted the pH of the system to 8-9 with sodium carbonate aqueous solution, added dropwise sodium borohydride water to disperse solution (100ml containing 80mmol of sodium borohydride) for reduction, continued stirring for 6-8h after the dropwise addition, then filtered and washed with water until there was no chloride ion in the filtrate, and vacuum-dried at 40°C to obtain a zinc-modified Pd catalyst supported on silicon carbide.

Embodiment 3

[0033] Catalyst performance evaluation is carried out on behalf of the zinc-modified Pd catalyst supported by silicon carbide prepared in Example 2, the method is as follows:

[0034] Substrate p-nitrophenylacetic acid (5mmol, 0.91g), catalyst (0.10g, ~10.0%wt), ammonium formate (20mmol, 1.26g) were reacted in 10ml methanol, and the substrate in the reaction solution was detected by HPLC after the reaction was finished. The conversion rate of p-nitrophenylacetic acid and the selectivity of product p-aminophenylacetic acid, the results are shown in table 1:

[0035] Table 1 catalyst catalytic performance

[0036] Reaction temperature / ℃

[0037] The test results show that the zinc-modified Pd catalyst supported by silicon carbide prepared by the invention can effectively catalyze the preparation of p-aminophenylacetic acid from p-nitrophenylacetic acid under heating conditions.

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Abstract

The invention belongs to the technical field of medicines and particularly relates to a preparation method of a medicine (actarit intermediate) for the rheumatic bone disease. The preparation method has the advantages that a zinc-modified Pd catalyst loaded with silicon carbide is obtained by firstly adopting nanosilicon nitride as a carrier and adopting zinc salt as a modifier to modify active Pd; by adoption of the zinc-modified Pd catalyst loaded with silicon carbide, p-nitrophenyl acetic acid can be effectively reduced to prepare p-aminophenyl acetic acid, and the reaction can be completely transformed by the catalyst with the use amount being several in ten thousandth of that of p-nitrophenyl acetic acid.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of an intermediate of Actarit, a medicine for rheumatic bone disease. Background technique [0002] Actarit, whose chemical name is 4-acetamidophenylacetic acid, is an immunomodulator developed by Japan's Nippon Shinyaku Company. It was first launched in Japan in 1994 and is mainly used clinically for the treatment of chronic rheumatoid arthritis. This product can inhibit and prevent the progressive destruction of articular bone and cartilage, activate T lymphocytes in patients, and enhance interleukin-2, thereby inhibiting allergic reactions. [0003] The molecular formula for p-aminophenylacetic acid is C 8 h 9 NO 2 , the CAS number is 1197-55-3, the molecular weight is 151.16, and its melting point is 199-200°C. P-aminophenylacetic acid is soluble in alcohol and lye, and slightly soluble in hot water. P-aminophenylacetic acid is often used ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/224B01J23/60B01J37/34B01J37/16C07C227/04C07C229/42
CPCB01J23/60B01J27/224B01J37/16B01J37/343C07C227/04C07C229/42
Inventor 董同宝
Owner ZIBO VOCATIONAL INST