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Preparation method of ethenzamide-saccharin eutectic crystal form II

A technology of ethyl salicylamine and crystal form, which is applied in the field of preparation of ethyl salicylamine-saccharin co-crystal, which can solve problems such as the inability to obtain pure co-crystal

Active Publication Date: 2014-12-03
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ethyl salicylamine-saccharin co-crystal is a typical asymmetric phase diagram system in commonly used alcohols and ketone solvents, and the pure co-crystal cannot be obtained by solution evaporation

Method used

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  • Preparation method of ethenzamide-saccharin eutectic crystal form II

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Embodiment 1

[0019] A preparation method of disalicylamine-saccharin co-crystal form II, comprising the following steps:

[0020] (1) Polish the aluminum substrate with a purity of 99.99% with 400# sandpaper, put it into ethanol for ultrasonic degreasing and cleaning for 5 minutes, take it out, put it into an aqueous sodium hydroxide solution with a mass concentration of 4% and clean it for 5 minutes, wash with water, and dry to obtain A layer of Al is formed on the surface 2 O 3 Thin-film aluminum substrate, named Al 2 O 3 / Al substrate; 2 O 3 / Al substrates were immersed in 10 mM eicosanic acid (CH 3 (CH 2 ) 18 COOH) in n-hexadecane solution, sealed at room temperature for surface self-assembly for 24 hours; the self-assembled substrate was rinsed with fresh n-hexane and then placed in anhydrous methanol for 10 minutes to be sonicated to remove surface physical adsorption and Deposited eicosanoic acid; washed with anhydrous methanol, dried at 50°C for 5h; put in 0.1M MgCl 2 Imme...

Embodiment 2

[0023] A preparation method of disalicylamine-saccharin co-crystal form II, comprising the following steps:

[0024] (1) Polish the aluminum substrate with a purity of 99.99% with 600# sandpaper, put it into acetone for ultrasonic degreasing and cleaning for 10min, take it out, put it into an aqueous sodium carbonate solution with a mass concentration of 8% for cleaning for 4min, wash with water, and dry to obtain the surface form a layer of Al 2 O 3 Thin-film aluminum substrate, named Al 2 O 3 / Al substrate; 2 O 3 / Al substrates were immersed in 50 mM tetradecanoic acid (CH 3 (CH 2 ) 12 COOH) in n-hexadecane solution, sealed at room temperature for surface self-assembly for 72 hours; the self-assembled substrate was rinsed with fresh n-hexane and then placed in anhydrous methanol for 10 minutes to be sonicated to remove surface physical adsorption and The deposited tetradecanoic acid; washed with anhydrous methanol, dried at 80°C for 3h; put in 0.8M AlCl 3 Immerse in...

Embodiment 3

[0028] A preparation method of disalicylamine-saccharin co-crystal form II, comprising the following steps:

[0029] (1) The aluminum substrate with a purity of 99.99% is polished with 500# sandpaper, put into ethanol for ultrasonic degreasing and cleaning for 6 minutes, taken out, put into an aqueous sodium hydroxide solution with a mass concentration of 8% for cleaning for 6 minutes, washed with water, and dried to obtain A layer of Al is formed on the surface 2 O 3 Thin-film aluminum substrate, named Al 2 O 3 / Al substrate; 2 O 3 / Al substrates were immersed in behenic acid (CH) at a concentration of 35 mM 3 (CH 2 ) 20 COOH) in n-hexadecane solution, sealed at room temperature for surface self-assembly for 36 hours; the self-assembled substrate was rinsed with fresh n-hexane and then placed in anhydrous methanol for 10 minutes to sonicate to remove surface physical adsorption and deposited CH 3 (CH 2 ) 20 COOH; washed with anhydrous methanol, dried at 70°C for 4h...

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Abstract

The invention discloses a preparation method of an ethenzamide-saccharin eutectic crystal form II, which comprises the following steps: (1) polishing an aluminum substrate with sand paper, cleaning, drying, and immersing in a fatty acid solution to perform surface self-assembly; cleaning and drying; impregnating in a MgCl2 water solution, cleaning and drying; and (2) preparing an ethenzamide-saccharin mixture into a mixed solution, fixing and putting one end of the substrate obtained in the step (1) into the mixed solution, covering the container opening, evaporating at room temperature until the precipitated ethenzamide-saccharin eutectic crystal is attached to the substrate and the ethenzamide and saccharin crystals settle to the container bottom, taking out the substrate, cleaning, drying, and taking down the ethenzamide-saccharin eutectic crystal from the substrate. Unimolecules generated by the self-assembly of the fatty acids on the aluminum surface are self-assembled to form the film, and interaction force between the film molecules and the pharmaceutical molecules directionally induces the growth of the eutectic crystal, so that the ethenzamide-saccharin eutectic crystal form II can be obtained within a wider concentration range.

Description

technical field [0001] The invention relates to a preparation method of ethylsalicylamine-saccharin cocrystal form II, belonging to the preparation technology of ethylsalicylamine-saccharin cocrystal. Background technique [0002] On the premise of not changing the pharmacological behavior of drugs, drug co-crystals are designed and synthesized by introducing a variety of active drug components with different functions. The difference between co-crystallization and conventional crystallization is that substances of different compositions and properties can be crystallized together to form a crystalline homogeneous mixture of multiple components, that is, a co-crystal. As a new solid form of today's drugs, co-crystals have unique physicochemical properties and bioavailability that are different from traditional drugs, and are a new direction for drug development. [0003] At present, some experts from Europe and the United States and other countries are actively engaged in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/60C07C231/24C07D275/06
Inventor 党乐平佟瑶张鹏王占忠卫宏远
Owner TIANJIN UNIV