Check patentability & draft patents in minutes with Patsnap Eureka AI!

Crystal compound of 4,5,6,7-tetrahydro-isoxazolo[5,4-c]pyridine-3-alcohol-hydrate

A monohydrate and compound technology, applied in organic chemistry, drug combination, respiratory diseases, etc., can solve the problems of organic impurities residues, affecting the bioavailability of crystalline compounds and drug safety, etc., to achieve simple operation and improved effect Obvious, low-yield effect

Inactive Publication Date: 2012-07-25
TIANJIN INSTITUTE OF PHARMA RESEARCH
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic solvent triethylamine is used as a necessary solvent in the crystal form preparation methods disclosed in these documents, and there is a problem of residual organic impurities, which will seriously affect the bioavailability and drug safety of the crystal form compound

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Crystal compound of 4,5,6,7-tetrahydro-isoxazolo[5,4-c]pyridine-3-alcohol-hydrate
  • Crystal compound of 4,5,6,7-tetrahydro-isoxazolo[5,4-c]pyridine-3-alcohol-hydrate
  • Crystal compound of 4,5,6,7-tetrahydro-isoxazolo[5,4-c]pyridine-3-alcohol-hydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1 Preparation of crystalline compounds

[0042] This example is the preparation method of the crystalline compound provided by the present invention, and the specific steps are as follows:

[0043] 1) Dissolve 1 g of 4,5,6,7-tetrahydroisoxazolo[5,4-c]pyridin-3-ol in 50 mL of water and heat to 60-100 °C;

[0044] 2) The solution was concentrated under reduced pressure until just a solid was precipitated, and the volume of the solution was about 20 mL at this time;

[0045] 3) Then heat it to 60-100°C to dissolve;

[0046] 4) Stand at room temperature for several days to crystallize, filter, collect the solid, and dry to obtain a white crystalline powder, which is the 4,5,6,7-tetrahydroisoxazolo[5,4-c] provided by the present invention Crystal form of pyridin-3-ol monohydrate.

[0047] The purity of the crystalline compound prepared by the above method is 99.95%, and the related substances are less than 0.1%.

[0048] According to the method of triethylamine...

Embodiment 2

[0049] Example 2 Identification of crystalline compounds

[0050] This example is the crystalline compound of 4,5,6,7-tetrahydroisoxazolo[5,4-c]pyridin-3-ol monohydrate prepared in Example 1 using the following methods for identification.

[0051] 1) X-ray diffraction

[0052] Use the Japanese Rigaku D / Max-2500 X-ray diffractometer to measure the specific structure of the crystalline compound prepared in Example 1. The specific experimental parameters are set as follows: CuKα radiation, tube voltage 40KV, tube current 100mA, 2θ angle scanning range is 2 ~40°, the scan speed is 8° / min. The X-ray diffraction pattern of this crystalline compound and the result data of its peak retrieval are as follows figure 1 As shown, the specific X-ray diffraction peak data are shown in Table 1.

[0053]

[0054] 2) Thermogravimetric analysis

[0055] The crystalline compound prepared in Example 1 was measured using a Japanese Rigaku standard TG-DTA thermogravimetric analyzer. The sp...

Embodiment 3

[0062] Example 3 Physicochemical properties of crystalline compounds

[0063] This example is the crystalline compound of 4,5,6,7-tetrahydroisoxazolo[5,4-c]pyridin-3-ol monohydrate prepared in Example 1, which has the following physical and chemical properties:

[0064] White crystalline powder, stable under high temperature, high humidity and strong light. Soluble in hot water, slightly soluble in methanol, ethanol, acetone, chloroform, ethyl acetate.

[0065] This example also measured the solubility of the crystalline compound prepared in Example 1 in water at 25°C, and compared the crystalline compound prepared twice according to the triethylamine method disclosed in CN1914212A, and the results are shown in the table 2.

[0066] Solubility of Table 2 Crystal Compounds

[0067] Solubility

[0068] It can be seen from the above table that the solubility of the crystalline compound prepared by the present invention is obviously better than that of the crystal...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a crystal compound of 4,5,6,7-tetrahydro-isoxazolo[5,4-c]pyridine-3-alcohol-hydrate, which does not comprise or comprises a small quantity of organic solvent impurities and is used for treating sleep disorder, a method for preparing the crystal compound, a medicinal composition which takes the crystal compound as an active ingredient, and the medicinal application of the crystal compound to the preparation of a medicament for treating sleep disorder. The crystal compound does not comprise residual impurity peaks of an organic solvent, so that the crystal compound has superior bioavailability and medicament safety compared with the prior art; and in the preparation process by using the preparation method, water is taken as the solvent, so that operation is easy and convenient, an improvement effect is remarkable, and an organic solvent is not left.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry. Specifically, the present invention relates to 4,5,6,7-tetrahydroisoxazolo[5,4-c]pyridin-3-ol- Hydrate crystal compound. The present invention also relates to a method for preparing the crystalline compound. The present invention also relates to a pharmaceutical composition comprising said crystal form as an active ingredient. The present invention also relates to the medical use of the crystal form in the preparation of medicines for treating sleep disorders. Background technique [0002] The ability to exist in different crystalline compound structures is known as polymorphism, which is known to occur in many organic compounds. These different crystal forms are called "polymorphs" and differ in their packing, geometric arrangement and other descriptive properties in the crystalline solid state. Different polymorphs of substances have different lattice energies, so they exhibit different ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D498/04A61K31/437A61P25/20A61P11/00A61P25/24A61P25/18
Inventor 黄淑云李兴伟郁伟文王景阳
Owner TIANJIN INSTITUTE OF PHARMA RESEARCH
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com