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Preparation method of hydroxychloroquine sulfate

A technology of hydroxychloroquine sulfate and hydroxychloroquine, which is applied in the direction of organic chemistry, can solve the problems of long reaction time, etc., and achieve the effects of simple operation, lower reaction temperature and high yield

Pending Publication Date: 2022-05-13
ZHANG JIA GANG VINSCE BIO PHARM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, the reaction time of this reaction process is 20-40h, and the reaction time is longer

Method used

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  • Preparation method of hydroxychloroquine sulfate
  • Preparation method of hydroxychloroquine sulfate
  • Preparation method of hydroxychloroquine sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Add 150g of 4,7-dichloroquinoline, 25g of phenol and 75ml of isopropanol into the three-necked flask in sequence, start stirring, heat up to 110°C, and dropwise add 148.5g of 5-(N-ethyl-N-2 Hydroxyethylamine)-2-pentylamine, the dropwise addition was completed within 70 minutes, and after the dropwise addition was completed, the reaction was incubated at 110° C. for 7 hours.

[0046] (2) After the TLC reaction is completed, phenol and isopropanol are concentrated under reduced pressure, and can be recycled in barrels. Cool down to below 30°C, add 800ml of dichloromethane and stir for 25 minutes, then add 400ml of 10% aqueous sodium hydroxide solution to make the pH = 11-12, stir for 25 minutes, let stand for 25 minutes to separate layers, leave the dichloromethane layer, and the water layer Discard it; add 200ml concentration of 35% hydrochloric acid to the dichloromethane layer to adjust the pH to 2-3, stir for 25 minutes, let stand for 25 minutes to separate layers...

Embodiment 2

[0049] Different from Example 1, in step (1), add 150ml Virahol, all the other are the same.

[0050] The obtained hydroxychloroquine in step (2) was 168.4 g, the yield was 66.16%, and the purity was 98.5%.

Embodiment 3

[0052] Different from Example 1, in step (1), add 75ml propanol, all the other are the same.

[0053] The obtained hydroxychloroquine in step (2) was 166.2 g, the yield was 65.29%, and the purity was 98.3%.

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Abstract

The invention discloses a preparation method of hydroxychloroquine sulfate, and belongs to the technical field of medicine synthesis. The method comprises the following steps: (1) mixing 4, 7-dichloroquinoline, an auxiliary agent and phenol, heating, adding a side chain, and reacting to obtain a hydroxychloroquine crude product; (2) purifying the hydroxychloroquine crude product obtained in the step (1) to obtain hydroxychloroquine; and (3) dissolving the hydroxychloroquine obtained in the step (2), and adding sulfuric acid to obtain hydroxychloroquine sulfate. The preparation method can shorten the reaction time, reduce the reaction temperature, reduce the generation of impurities, greatly reduce the production cost and reduce the environmental pollution, and is simple to operate and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical synthesis, and in particular relates to a preparation method of hydroxychloroquine sulfate. Background technique [0002] Hydroxychloroquine (HCQ) and chloroquine, which are antimalarial drugs, have been used clinically as important drugs for the treatment of rheumatic diseases such as systemic lupus erythematosus (SLE) and rheumatoid arthritis (RA). Due to the recognition of the extensive role of hydroxychloroquine in immune regulation, it has become a research hotspot, and the role of hydroxychloroquine in the treatment of rheumatism has also attracted more and more attention. The latest research shows that hydroxychloroquine sulfate is a slow-acting antirheumatic drug that is safe, effective and well tolerated. Hydroxychloroquine Sulfate (Hydroxychloroquine Sulfate), the chemical name is 2-[[4-[(7-chloro-4-quinolyl)amino]pentyl]ethylamino]-ethanol sulfate is a quinoline drug, clinical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/46
CPCC07D215/46
Inventor 彭学东张梅赵金召
Owner ZHANG JIA GANG VINSCE BIO PHARM
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