Hydroxychloroquine sulfate hydrate as well as crystal form, preparation method and application thereof

A technology of hydroxychloroquine sulfate and hydrate, applied in the field of hydroxychloroquine sulfate hydrate, can solve problems such as poor hygroscopicity, and achieve the effects of stable and reliable quality, simple and feasible preparation method, and good prospect of finished medicine

Pending Publication Date: 2021-11-05
SHANGHAI ZHONGXI SUNVE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by this invention is to provide a kind of hydroxychloroquine sulfate hydrate, its crystal form and its preparation method in order to overcome the defect of poor hygroscopicity of the crystal form of hydroxychloroquine sulfate in the prior art

Method used

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  • Hydroxychloroquine sulfate hydrate as well as crystal form, preparation method and application thereof
  • Hydroxychloroquine sulfate hydrate as well as crystal form, preparation method and application thereof
  • Hydroxychloroquine sulfate hydrate as well as crystal form, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] Embodiment 1: the preparation of hydroxychloroquine sulfate amorphous

[0089] Take 3g of crystal form A of hydroxychloroquine sulfate (synthesized according to Example 2 of patent CN108727263A), add 9mL of 2,2,2-trifluoroethanol and stir to dissolve, place it on a rotary evaporator and steam it, and set the temperature to 60 °C, the rotational speed was set at 100 rpm, and the title product was obtained after spin-drying. The XRPD detection product is an amorphous state, and its XRPD spectrum is as follows figure 1 shown.

Embodiment 2

[0090] Embodiment 2: Preparation of the crystal form B of hydroxychloroquine sulfate monohydrate

[0091] Take 300 mg of amorphous hydroxychloroquine sulfate prepared in Example 1, add m-xylylene dimethyl ether 8 mL (water containing impurities, water content is 0.1 wt%), place on a shaker, 25 ° C, 250 rpm, shake for 48 hours and then filter. The filtered sample was dried in a vacuum oven (vacuum degree -0.1 MPa) at 35 °C for 24 h to obtain the title product. The product detected by XRPD is crystal form B, and the peak width and peak height relative intensity in the X-ray powder diffraction pattern represented by 2θ angle are as follows:

[0092]

[0093]

[0094] XRPD spectrum as figure 2 shown.

[0095] DSC spectrum such as image 3 shown.

[0096] TGA spectrum as Figure 4 As shown, it shows that the corresponding weight loss of the sample is 4.140% before 150°C. According to the molecular weight of hydroxychloroquine sulfate, the ratio of hydroxychloroquine sul...

Embodiment 3

[0099] Embodiment 3: the preparation of the crystal form B of hydroxychloroquine sulfate monohydrate

[0100] Take 300 mg of amorphous hydroxychloroquine sulfate prepared in Example 1, add 8 mL of 3-methyl-1-butanol (water containing impurities, water content is 0.1 wt%), place on a shaker, 25 ° C, 250 rpm, and shake for 24 h After filtering. The filtered sample was dried in a vacuum oven (vacuum degree -0.1 MPa) at 35 °C for 24 h to obtain the title product. The product detected by XRPD is the crystal form B of hydroxychloroquine sulfate monohydrate, and its identification data is basically the same as in Example 2.

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Abstract

The invention discloses a hydroxychloroquine sulfate hydrate as well as a crystal form, a preparation method and application thereof. The hydroxychloroquine sulfate hydrate, especially the crystal forms B, C and D of the hydrate, has better moisture absorption stability, is easy for industrial production and subsequent preparation operation, is stable and reliable in quality, and has better patent medicine prospects.

Description

technical field [0001] The invention relates to hydroxychloroquine sulfate hydrate, its crystal form, its preparation method and application. Background technique [0002] Hydroxychloroquine Sulfate, chemical name: 2-[[4-[(7-chloro-4-quinolyl)amino]pentyl, ethylamino]ethanol sulfate, CAS number: 747-36-40 . Hydroxychloroquine sulfate was developed by Winthrop Company and was first launched in the United States in 1956. It has been 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. Due to its unique mechanism of action and good safety, hydroxychloroquine sulfate is more and more widely used in the field of rheumatism. After the 1990s in the 20th century, more than 90% of clinical treatments for rheumatism all selected hydroxychloroquine sulfate, and its structure is as follows: [0003] [0004] Patent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/46A61K31/4706A61P37/02A61P29/00A61P19/02
CPCC07D215/46A61P37/02A61P29/00A61P19/02C07B2200/13
Inventor 颜国明洪鸣凰齐明辉任国宾尹超俞伟李杰
Owner SHANGHAI ZHONGXI SUNVE PHARMA
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