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High-purity gentisic acid and application thereof

A gentisic acid, high-purity technology, applied to high-purity gentisic acid and its application field, can solve the problems of poor product purity and low yield of gentisic acid

Pending Publication Date: 2022-06-17
BEIJING SINOTAU INT PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The gentisic acid product purity that each method of above-mentioned prior art obtains is all poor, and yield is all low

Method used

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  • High-purity gentisic acid and application thereof
  • High-purity gentisic acid and application thereof
  • High-purity gentisic acid and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0167] Feeding reaction: add 5.0mol / L NaOH solution to the reaction kettle, add 50g of 5-bromosalicylic acid, 0.5g of cuprous iodide, and 0.5g of oxalic acid; under nitrogen protection, start stirring; heat up to 100~120℃ for 24h, Sampling control HPLC (5-bromosalicylic acid)≤1.5%; cool down to 20~30℃, add water;

[0168] Acidification: control the temperature to 20~30℃, add concentrated hydrochloric acid to adjust the pH of the reaction solution to (2.4), there is solid precipitation, filter;

[0169] Extraction: add 50 g of sodium chloride and 250 g of methyl tert-butyl ether to the filtrate, stir and extract, and flocs appear after standing;

[0170] Filtration: 5 g of diatomaceous earth was added to the Buchner funnel, filtered and separated to obtain the first organic phase and the aqueous phase; 125 g of methyl tert-butyl ether was added to the aqueous phase, filtered and separated to obtain the second organic phase. 2 and organic phase 1 are combined to obtain organic ...

Embodiment 2

[0177] Feeding reaction: add 5.0mol / L NaOH solution to the reaction kettle, add 200g of 5-bromosalicylic acid, 1.8g of cuprous chloride, and 2g of oxalic acid; under nitrogen protection, turn on stirring; heat up to 100~120℃ for 24h reaction, take samples In-control HPLC (5-bromosalicylic acid)≤1.5%; cool down to room temperature (20~30℃), add water;

[0178] Acidification: control the temperature to 20~30℃, add concentrated hydrochloric acid to adjust the pH of the reaction solution to 2.4, there is solid precipitation, and filter;

[0179] Extraction: add 200 g of sodium chloride and 1000 g of methyl tert-butyl ether to the filtrate, stir and extract, and flocs appear after standing;

[0180] Filtration: add 50 g of diatomaceous earth to the Buchner funnel, filter, and separate the liquids to obtain an organic phase 1 and an aqueous phase; add 500 g of methyl tert-butyl ether to the aqueous phase, filter, and separate liquids to obtain an organic phase 2. 2 and organic phase ...

Embodiment 3

[0187] Feeding reaction: add 5.0mol / L KOH solution to the reaction kettle, add 500 g of 5-bromosalicylic acid, 5.0 g of copper sulfate pentahydrate, and 5 g of oxalic acid; under nitrogen protection, start stirring; heat up to 100~120 ° C for 24 hours, and take samples In-control HPLC (5-bromosalicylic acid)≤1.5%; cool down to room temperature (20~30℃), add water;

[0188] Acidification: control the temperature to 20~30℃, add concentrated hydrochloric acid to adjust the pH of the reaction solution to 2.4, there is solid precipitation, and filter;

[0189] Extraction: Add 500 g of sodium chloride and 250 g of methyl tert-butyl ether to the filtrate, stir and extract, and flocs appear after standing;

[0190] Filtration: add 50 g of diatomaceous earth to the Buchner funnel, filter, and separate the liquids to obtain an organic phase 1 and an aqueous phase; add 125 g of methyl tert-butyl ether to the aqueous phase, filter, and separate liquids to obtain an organic phase 2. 2 and...

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Abstract

The invention discloses high-purity gentisic acid, the purity of the high-purity gentisic acid is greater than or equal to 99.50%, the high-purity gentisic acid comprises gentisic acid, salicylic acid and an impurity A, and the structural formula of the impurity A is shown in the specification. The invention also discloses an application of the high-purity gentisic acid in preparation of an antiviral agent, an antibacterial agent, an analgesic or an antioxidant excipient. The high-purity gentisic acid is prepared through a specific preparation method, the yield of the high-purity gentisic acid can reach 18-22%, and the high-purity gentisic acid is suitable for large-scale industrial production.

Description

technical field [0001] The present application relates to the field of medicine and chemical industry. Specifically, the present application relates to a high-purity gentisic acid and applications thereof. Background technique [0002] Gentianic acid, chemical name 2,5-dihydroxybenzoic acid, also known as 5-hydroxysalicylic acid, is a secondary product of salicylic acid after renal metabolism, and is commonly used clinically as an antiviral, antibacterial and analgesic agent (sodium salt). Gentianic acid is a hydroquinone compound that is prone to oxidation reaction and is also used as an antioxidant excipient in the pharmaceutical industry. Gentianic acid has been used as a pharmaceutical excipient in foreign countries. [0003] In the prior art, benzoic acid is used as a raw material to synthesize products through steps such as chlorination and hydrolysis, but there are five main products synthesized by this method, and the products are difficult to separate and purify,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/05C07C51/487C07C51/02C07C51/48C07C51/43C07C51/41C07C51/47A61P31/12A61P31/04A61P29/00A61P39/06A61P25/04
CPCC07C65/05C07C51/487C07C51/02C07C51/48C07C51/43C07C51/412C07C51/47A61P31/12A61P31/04A61P29/00A61P39/06A61P25/04
Inventor 颜寒郑策何立涛
Owner BEIJING SINOTAU INT PHARMA TECH CO LTD
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