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Novel preparation method of hydroxychloroquine sulfate

A technology of hydroxychloroquine sulfate and hydroxychloroquine, which is applied in the field of medicine and chemical industry, can solve the problems affecting the purification of hydroxychloroquine free base, high difficulty in operation, and difficult removal, so as to reduce production cost and pollution control cost, and the post-processing is simple and avoids The effect of impurity inclusion

Inactive Publication Date: 2019-03-12
南京天际联盟医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under high temperature conditions, sodium alkoxide will undergo nucleophilic substitution with 4,7-dichloroquinoline to generate ether products, which are not easy to remove, which affects the purification of hydroxychloroquine free base, and the alcoholic hydroxyl group on the side chain is in the presence of sodium alkoxide. In the presence of it, hydroxyl anions will be formed, and by-products will be formed with 4,7-dichloroquinoline, which will make purification difficult, and the reaction must control the heating process and solvent evaporation speed, which is difficult to operate

Method used

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  • Novel preparation method of hydroxychloroquine sulfate
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  • Novel preparation method of hydroxychloroquine sulfate

Examples

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Embodiment 1

[0036] Example 1: Preparation of potassium fluoride supported on alumina

[0037] Dissolve 10g of anhydrous potassium fluoride and 30g of 200-mesh alumina powder in 100ml of water, stir ultrasonically at 50 Hz for 45 minutes, evaporate the water under reduced pressure at 55°C to obtain a solid powder, dry it in vacuum at 120°C for 8 hours, take it out, and grind it into a powder After that, 40 g of catalyst was obtained.

Embodiment 2

[0038] Example 2: Preparation of tetrabutylammonium fluoride supported on alumina

[0039] Dissolve 40g of tetrabutylammonium fluoride and 40g of 200-mesh alumina powder in 100ml of water, stir ultrasonically at 50 Hz for 45 minutes, evaporate the water to dryness under reduced pressure at 55°C to obtain a solid powder, dry it in vacuum at 130°C for 8 hours, remove it, and grind it into powder to obtain 80 g of catalyst.

Embodiment 3

[0040] Embodiment 3: Preparation of cesium fluoride supported on alumina

[0041] Dissolve 10g of cesium fluoride and 20g of 200-mesh alumina powder in 100ml of water, stir ultrasonically at 50 Hz for 1 hour, evaporate the water under reduced pressure at 55°C to obtain a solid powder, dry it in vacuum at 100°C for 4 hours, take it out, and grind it into a powder , to obtain 30g catalyst.

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Abstract

The invention discloses a preparation method of hydroxychloroquine sulfate. The preparation method is characterized in that a parent core 4,7-dichloroquinoline used as a starting material and a hydroxychloroquine side chain 5-(N-ethyl-N-2- ethanolamine)-2-amylamine undergo condensation reaction in the presence of a catalyst to obtain a hydroxychloroquine free base, and then the hydroxychloroquinefree base undergoes salt formation with sulfuric acid to obtain the hydroxychloroquine sulfate. The preparation method overcomes the disadvantages in the prior art, and has the advantages that the useamount of the side chain is reduced; the total yield is more than or equal to 90 percent; the yield of the hydroxychloroquine sulfate is more than or equal to 96 percent; the total yield is more thanor equal to 86 percent; the purity of the hydroxychloroquine sulfate is more than 99. 7 percent; and the single impurity is less than 0.1 percent. The preparation method meets the pharmacopoeia requirements and is short in reaction time, easy and convenient to operate, low in pollution, low in cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and specifically designs hydroxychloroquine sulfate, which is a medicine for treating discoid lupus erythematosus and systemic lupus erythematosus. Background technique [0002] Hydroxychloroquine Sulfate (Hydroxychloroquine Sulfate, HCQ) chemical name is 2-[[4-[(7-chloro-4-quinolyl)amino]pentyl]ethylamino]-ethanol sulfate, CAS number is 747-36- 4. The chemical structure is as follows: [0003] [0004] Hydroxychloroquine sulfate was successfully developed by Winthrop Company. It was first listed in the United States in 1956, and then listed in France, Denmark, Japan, Germany, Finland and other countries and regions. U.S. FDA approved hydroxychloroquine sulfate tablets on May 29, 1998 for the treatment of lupus erythematosus and rheumatoid arthritis. [0005] US2546658 discloses a kind of synthetic method of hydroxychloroquine sulfate, and the reaction process of this ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/46
CPCC07D215/46
Inventor 强浩徐强殷勇
Owner 南京天际联盟医药科技有限公司
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