Dapagliflozin hemihydrate, crystal form of dapagliflozin hemihydrate, preparation method of crystal form of dapagliflozin hemihydrate and pharmaceutical composition

A hemihydrate and composition technology, which is applied in the field of dapagliflozin hemihydrate and its crystal form, can solve the problems of long preparation time, expensive propylene glycol, and inability to maintain the original crystal form, and achieve cheap solvents and easy preparation The effect of simple method

Active Publication Date: 2016-11-23
SOLIPHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The present inventors have disclosed the dapagliflozin amorphous substance and the dapagliflozin hydrate crystal form A, the dapagliflozin hydrate crystal form B, and the dapagliflozin (S)-propylene glycol monohydrate disclosed in the above documents. Repeated tests and property tests were carried out, and the results showed that: the known amorphous form of dapagliflozin is easy to absorb moisture into oil or transform into other hydrate crystal states; the known crystal form of dap

Method used

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  • Dapagliflozin hemihydrate, crystal form of dapagliflozin hemihydrate, preparation method of crystal form of dapagliflozin hemihydrate and pharmaceutical composition
  • Dapagliflozin hemihydrate, crystal form of dapagliflozin hemihydrate, preparation method of crystal form of dapagliflozin hemihydrate and pharmaceutical composition
  • Dapagliflozin hemihydrate, crystal form of dapagliflozin hemihydrate, preparation method of crystal form of dapagliflozin hemihydrate and pharmaceutical composition

Examples

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Example Embodiment

[0074] Preparation Example 1 (Preparation of known dapagliflozin amorphous)

[0075] The known dapagliflozin amorphous can be prepared according to the method described in the patent document US6515117B2 or prepared according to the following method.

[0076] Take 40 mg of dapagliflozin oil, add 400 microliters of dichloromethane to dissolve, and spin dry at room temperature to obtain a white foamy dapagliflozin amorphous.

Example Embodiment

[0077] Preparation Example 2 (Preparation of known dapagliflozin amorphous)

[0078] Take 500 mg of Dapagliflozin oil, add 5 ml of dichloromethane to dissolve, and spin to dry at room temperature to obtain part of the oil and part of the foamy solid to mix. Add 5 ml of n-heptane, stir at room temperature for 4 hours, filter under reduced pressure, and vacuum dry the filter cake at room temperature for 24 hours to obtain dapagliflozin amorphous.

[0079] XRPD diagram see figure 1 , appearing as amorphous.

Example Embodiment

[0080] Preparation Example 3 (Preparation of known dapagliflozin dihydrate crystal form A)

[0081] The known dapagliflozin dihydrate crystal form A can be prepared according to the method described in Example 3 of the patent document CN103958491A or according to the following method.

[0082] The specific preparation method is as follows: take 50 mg of amorphous dapagliflozin prepared in Preparation Example 2, suspend it in 3 ml of water, and heat it to 80°C. To this mixture was added a solution of 20 mg of xylitol in 0.5 ml of water to form an emulsion, which was cooled to 5°C at a rate of 2°C per hour. At this temperature, the mixture was stirred for about 20 hours or until crystals could be detected by optical microscopy. After crystallization, the suspension was filtered and the solid product was dried in air at room temperature at about 50% relative humidity for about 1 hour to yield Dapagliflozin dihydrate Form A.

[0083] XRPD diagram see figure 2 , shown to be c...

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Abstract

The invention relates to a dapagliflozin hemihydrate and a crystal form C thereof. Compared with the prior art, the dapagliflozin hemihydrate and the crystal form C thereof have high stability in water or a water-containing system and are more suitable for being treated with the wet granulation technology or being prepared into suspension. The invention further relates to a preparation method of the crystal form C of the dapagliflozin hemihydrate.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical crystals. Specifically, it relates to dapagliflozin hemihydrate, its crystal form, and a preparation method. Background technique [0002] Dapagliflozin (trade name: Farxiga) is a sodium-glucose cotransporter-2 (SGLT2) inhibitor, which can reduce the glucose in the renal tubules by making it unable to reabsorb smoothly into the blood and excreted with the urine. Blood glucose concentration, indicated in adults with type 2 diabetes as an adjunct to diet and exercise to improve glycemic control. Daxigliflozin was jointly developed by AstraZeneca and Bristol-Myers Squibb. The drug was approved by the European Commission for the treatment of type 2 diabetes in adults on November 12, 2012. It is also the world's first SGLT2 drug. an approved drug. The U.S. Food and Drug Administration (FDA) refused approval in January 2012 on the grounds that it may cause breast and bladder cancer safety issu...

Claims

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Application Information

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IPC IPC(8): C07D309/10A61K31/351A61P3/10A61P3/06A61P25/00A61P27/02A61P13/12A61P17/02A61P5/50A61P3/04A61P3/00A61P9/10A61P9/12
Inventor 汪晶盛晓霞
Owner SOLIPHARMA
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