Unlock instant, AI-driven research and patent intelligence for your innovation.
Preparation method of glimepiride crystal form I
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology of glimepiride and crystal form, which is applied in the field of raw material drug preparation, can solve the problems that glimepiride is easy to degrade, deteriorate, change color, exceed the standard, and has no practical value.
Active Publication Date: 2019-09-10
迪嘉药业集团股份有限公司
View PDF4 Cites 2 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
[0009] Experiments have found that crystal form I is relatively easy to obtain, but it is very easy to cause solvent wrapping during the crystallization process. The solvent wrapped in this kind of wrapping is very stable. It can be dried by drying, increasing the drying time, vacuum drying, and drying after airflow crushing. cannot be removed or reduced to acceptable limits (ICH Q3C limit standard)
[0010] After experiments, the crystal form II
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
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0037] Example 1 (ethanol)
[0038] With 13.0g of crude glimepiride, add 130g of 95% ethanol, 4.18g of 27% ammonia water, and 25g of water, stir and dissolve, dissolve, filter, and slowly add 4.38g of glacial acetic acid (diluted with 26g of water) to the filtrate, dropwise After completion, continue to stir for 1 hour, filter, wash with water, and dry at 70°C to obtain 12.27g of the product, yield: 94.4%. It was determined to be crystal form II by XRD detection.
Embodiment 2
[0039] Example 2 (n-propanol)
[0040] Add 10.0g of glimepiride crude product, 100g of n-propanol, 3.21g of 27% ammonia water, and 20g of water, stir to dissolve, dissolve, filter, and slowly add 3.37g of glacial acetic acid (diluted with 20g of water) to the filtrate, dropwise After completion, continue to stir for 1 hour, filter, wash with water, and dry at 70°C to obtain 8.47g of the product with a yield of 84.7%. It was determined to be crystal form II by XRD detection.
Embodiment 3
[0041] Example 3 (isopropanol)
[0042] Add 5.0 g of crude glimepiride, 30 g of isopropanol, 10 g of purified water, and 1.61 g of 27% ammonia water, stir to dissolve, dissolve, filter, and slowly add 1.68 g of glacial acetic acid (diluted with 10 g of water) to the filtrate, dropwise After completion, continue to stir for 1 hour, filter, wash with water, and dry at 70°C to obtain 4.65 g of the product, yield: 93.0%. It was determined to be crystal form II by XRD detection.
[0043] Preparation of crystal form I by transcrystallization
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
Login to View More
Abstract
The invention relates to a preparation method of glimepiride crystal form I, belonging to the technical field of preparation of active pharmaceutical ingredient. The preparation method of the glimepiride crystal form I comprises the following steps: dissolving the crude glimepiride in an aqueous solution of alcohol, adding an appropriate amount of ammonia water, and stirring and dissolving the crude glimepiride; filtering, adding acetic acid to the filtrate, neutralizing ammonia in the filtrate, and obtaining glimepiride crystal form II; adding a ketone solvent with the weight of 4-8 times that of the crystal form II, stirring for more than 10 hours at the temperature range of 10-35 DEG C, filtering, and drying at 70 DEG C to obtain the glimepiride crystal form I. The invention obtains high-quality glimepiride crystal form I active pharmaceutical ingredient.
Description
technical field [0001] The invention relates to a preparation method of glimepiride crystal form I, which belongs to the technical field of preparation of raw materials. Background technique [0002] Glimepiride (compound of formula I), as a novel sulfonamide hypoglycemic drug, is used for the treatment of type 2 diabetes. Foreign studies have found that it has a strong extramembrane hypoglycemic effect, including increasing insulin sensitivity and simulating the action of peripheral insulin, improving the translocation / dephosphorylation of glucose transporter (GLUT-4), and increasing the concentration of glucose in peripheral tissues. ingest. Among all sulfonamides, glimepiride has the lowest ratio of plasma insulin rise to blood glucose fall. [0003] [0004] The common forms of glimepiride are: amorphous, crystal form I, crystal form II, domestic reports of α, β, γ, δ, ε and other crystal forms. Among them, crystal form I is a pharmaceutical crystal form, which is ...
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
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to View More 
Login to View More 
