Preparation method of glimepiride crystal form I

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 ...

AI Technical Summary

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

Images