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Vanilline crystal form as well as preparation method and application thereof

A technology of vanillin and crystal form, which is applied in the field of vanillin crystal form and its preparation, can solve problems such as differences in drug dissolution and bioavailability, influence on drug absorption and utilization, and difference in drug solubility, so as to meet the requirements of bioavailability and drug solubility. Effectiveness requirements, avoiding changes in bioavailability and drug efficacy, and effects that are not easily affected by humidity

Inactive Publication Date: 2019-03-22
药大制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Different crystal forms of the same drug often lead to differences in drug solubility, which can cause differences in drug dissolution and bioavailability, thereby affecting the absorption and utilization of drugs in the body, and then resulting in differences in drug efficacy

Method used

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  • Vanilline crystal form as well as preparation method and application thereof
  • Vanilline crystal form as well as preparation method and application thereof
  • Vanilline crystal form as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Add 100g of vanillin, 630mL of water, and 63mL of ethanol into the reaction flask in sequence, raise the temperature to 75-85°C until clarification, remove insoluble matter by suction filtration while it is hot; heat the filtrate again until clarification, cool down to 10±5°C to crystallize for 6-8 Hour. Suction filtration, wash the filter cake (50mL×2). The filter cake was vacuum dried at 60°C to constant weight. 85.1 g of white crystals were obtained, the HPLC purity was 99.97%, and the yield was 85.1%.

[0056] Gained crystal carries out X-ray powder diffraction (XRPD) analysis (see appendix figure 1 ), DSC analysis (see attached figure 2 ) and TGA analysis (attached image 3 ). The results indicated Form A.

Embodiment 2

[0058] Add 100g of vanillin, 500mL of water, and 100mL of ethanol into the reaction flask in sequence, raise the temperature to 75-85°C until clarified, remove insoluble matter by suction filtration while it is hot; heat the filtrate again until clarified, cool down to 10±5°C to crystallize for 6-8 Hour. Suction filtration, wash the filter cake (50mL×2). The filter cake was vacuum dried at 60°C to constant weight. 80.5 g of crystal form A was obtained, the HPLC purity was 99.92%, and the yield was 80.5%.

Embodiment 3

[0060]Add 100g of vanillin, 700mL of water, and 70mL of acetone into the reaction flask in sequence, raise the temperature to 60-70°C until clarified, remove insoluble matter by suction filtration while it is hot; heat the filtrate again until clarified, cool down to 10±5°C to crystallize for 6-8 Hour. Suction filtration, wash the filter cake (50mL×2). The filter cake was vacuum dried at 60°C to constant weight. 88.9 g of crystal form A was obtained, the HPLC purity was 99.96%, and the yield was 88.9%.

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Abstract

The invention discloses a vanilline crystal form and a preparation method thereof. The vanilline crystal form is named a crystal form A. In an X-ray powder diffraction spectrum detected by using Cu-Kalpha radiation, characteristic peaks exit at the positions of 11.366, 11.740, 13.019, 13.894, 14.406, 17.187, 21.013, 21.685, 22.883, 23.778, 25.878, 26.59, 26.856, 28.638, 29.705+ / -0.2 <o> (2 theta). The invention also provides the preparation method of the vanilline crystal form A. The preparation method is simple and high in reproducibility; and the obtained vanilline crystal A is high in stability, high in purity and good in digesting performance, has no hygroscopicity, and is applicable to industrial production.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a vanillin crystal form and a preparation method and application thereof. Background technique [0002] Vanillin has another name called vanillin, and its chemical name is 3-methoxy-4-hydroxybenzaldehyde, and its structural formula is as shown in formula (I). [0003] [0004] Vanillin is the aroma component of the vanilla bean. Exist in beet, vanilla bean, benzoin gum, Peru balsam, Tuolu balsam, etc. It is a widely used edible spice. [0005] In addition, pharmacological tests have shown that vanillin can resist convulsions caused by pentylenetetrazol, inhibit epileptiform discharges, and inhibit spontaneous activities of animals, and has antiepileptic effects. At present, it has been developed as an antiepileptic drug for petit mal seizures, as well as an adjuvant drug for various types of epilepsy. [0006] Different crystal forms of the same drug often lead to differ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/58C07C45/81A61P25/08A61P25/14A61P25/00A61K31/11
CPCA61P25/00A61P25/08A61P25/14C07B2200/13C07C47/58
Inventor 王卉李志裕王举波王国保
Owner 药大制药有限公司
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