Hydroxychloroquine sulfate crystal form B and preparation method thereof

A technology of hydroxychloroquine sulfate crystals and hydroxychloroquine, applied in organic chemical methods, pharmaceutical formulations, medical preparations containing active ingredients, etc., can solve the problems of poor hygroscopicity, storage stability and low solubility, and achieve hygroscopicity Small size, improved physical and chemical properties, and good stability

Inactive Publication Date: 2021-03-12
NANJING HEALTHNICE MEDICAL TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydroxychloroquine sulfate crystal form A obtained by this patent has better thermal stability, but poor hygroscopicity, low storage stability and solubility

Method used

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  • Hydroxychloroquine sulfate crystal form B and preparation method thereof
  • Hydroxychloroquine sulfate crystal form B and preparation method thereof
  • Hydroxychloroquine sulfate crystal form B and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The preparation of embodiment 1 hydroxychloroquine sulfate crystal form B

[0036] Add 1100g of hydroxychloroquine and 8800ml of ethanol into the reaction flask, stir until dissolved, and control the temperature at 5-10°C. 330 g of 70% sulfuric acid aqueous solution was added dropwise, and the temperature was controlled not to exceed 10°C. After the dropwise addition, keep stirring at 5-10° C. for 12 h, filter, and vacuum-dry at 50° C. to constant weight to obtain 1401.2 g of hydroxychloroquine sulfate in crystal form B, with a yield of 98.6% and an HPLC purity of 99.93% (see figure 1 , XRD pattern see figure 2 , HPLC spectrum see image 3 ).

[0037] The preparation of comparative example 1 hydroxychloroquine sulfate A crystal form

[0038] Add 1100g of hydroxychloroquine and 880ml of ethanol into the reaction flask, stir until dissolved, and control the temperature at 35-40°C. Add 330 g of sulfuric acid aqueous solution with a mass fraction of 70% dropwise, and ...

Embodiment 2

[0041] Embodiment 2 investigates the test of the stability of hydroxychloroquine sulfate crystal form

[0042] 1. Influencing factor experiment

[0043] Carry out the influence factor test of this product and the crystal form in comparative example 1 and comparative example 2 according to (Chinese Pharmacopoeia 2015 edition two appendix XIX C) relevant regulations.

[0044] (1) High temperature test: take a proper amount of the test product and place it in a temperature-adjusting and humidity-adjusting box, and place it at 60°C for 60 days, and take samples on the 5th, 10th, 30th and 60th day, and focus on the investigation according to the stability The project requires testing.

[0045] Table 1 High temperature test results

[0046]

[0047] (2) High humidity test: take a proper amount of the test product and place it in a temperature-adjusting and humidity-adjusting box, and place it at 25°C under the condition of relative humidity of 90%±5% for 5 days, 10 days, 30 day...

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Abstract

The invention belongs to the technical field of medicinal chemistry, and particularly relates to a hydroxychloroquine sulfate crystal form B and a preparation method thereof, and XRD and DSC are usedfor characterization. The hydroxychloroquine sulfate crystal form B provided by the invention is simple in preparation method, low in hygroscopicity, good in stability, capable of forming a regular crystal form and higher in solubility, thereby being beneficial to process treatment of medicines, improvement of physical and chemical properties and improvement of patent medicine properties.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a hydroxychloroquine sulfate crystal form B and a preparation method thereof. Background technique [0002] Hydroxychloroquine Sulfate (Hydroxychloroquine Sulfate, HCQ), chemical name: 2-[[4-[(7-chloro-4-quinolyl)amino]pentyl]ethylamino]-ethanol sulfate. Successfully developed by Winthrop Company, it was first listed in the United States in 1956, and was approved by FDA on May 29, 1998. It is used for the treatment of lupus erythematosus and rheumatoid arthritis. Its chemical structure is as follows: [0003] [0004] Discoid lupus erythematosus (DLE) is a relatively common skin and mucous membrane connective tissue disease, 25% to 35% have oral lesions, which can be single in the oral cavity without skin lesions, and most of them have no obvious systemic symptoms. Its etiology and pathogenesis are still unclear, and it is difficult to treat, and it is prone to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/46A61K31/4706A61P37/02A61P19/02
CPCC07D215/46A61P37/02A61P19/02C07B2200/13
Inventor 辛妮王华娟
Owner NANJING HEALTHNICE MEDICAL TECH
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