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

Alogliptin benzoate impurity as well as preparation method and detection method thereof

A detection method, the technology of benzoic acid, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of controlling the content of impurities, no impurities, and potential safety hazards of alogliptin benzoate, etc., achieving good repeatability and simple preparation process , the effect of good application prospects

Pending Publication Date: 2021-09-28
成都伊诺达博医药科技有限公司
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, at present, there is no public literature or patent report on the impurities produced during the synthesis of alogliptin benzoate, and there is no reference substance for the impurities, so it is impossible to accurately control the impurities in the process route for the synthesis of alogliptin benzoate raw materials content, which brings safety hazards to alogliptin benzoate

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
  • Alogliptin benzoate impurity as well as preparation method and detection method thereof
  • Alogliptin benzoate impurity as well as preparation method and detection method thereof
  • Alogliptin benzoate impurity as well as preparation method and detection method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1, the synthesis of alogliptin benzoate impurity (impurity I) of the present invention

[0059]6-Chloro-3-methyluracil (3.2g, 0.02mol), 2-cyanobenzyl bromide (8.6g, 0.044mol), triethylamine (5.06g, 0.05mol) and N-methylpyrrolidone ( 20ml) into the reaction flask, heated to 80°C for 4.5h. Cool down to room temperature, add 30ml of water, and filter to obtain a crude product. Add 20ml of isopropanol, stir and beat at room temperature for 1h, filter, and dry to obtain impurity I (6.8g), with a yield of 87% and a purity of 97.2%. The data characterization spectrum of impurity I is as follows figure 1 and figure 2 As shown, the data characterization results are analyzed as follows:

[0060] 1 H-NMR (400MHz, CDCl 3 ):δ3.436(3H,s),4.151(2H,s),5.568(2H,s),7.249-7.334(3H,m),7.411-7.449(1H,m),7.480-7.522(1H,m ),7.584-7.636(2H,m),7.693-7.715(1H,m).

[0061] LCMS: m / z 391.1 [M+H] +

[0062]

Embodiment 2

[0063] Embodiment 2, the impurity I prepared by the present invention is used as reference substance to carry out quality control research on alogliptin benzoate medicine

[0064] The alogliptin benzoate impurity (impurity I) prepared in Example 1 was used as a reference substance to carry out quality control research on alogliptin benzoate medicines.

[0065] Alogliptin benzoate is prepared according to the method described in WO2005095381A1.

[0066] The HPLC detection condition of alogliptin benzoate impurity of the present invention is as shown in table 1:

[0067] Table 1. The HPLC detection condition of alogliptin benzoate impurity of the present invention

[0068]

[0069] 1. The distinction between alogliptin benzoate and impurity I

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 an alogliptin benzoate impurity as well as a preparation method and a detection method thereof, and belongs to the field of medicine quality control. The structural formula of the impurity is shown as a formula I. The invention also provides a preparation method of the impurity. The purity of the impurity I prepared by the invention is 97.2%, and meets the quality requirements of impurity reference substances related to the national pharmacopoeia and the Chinese pharmacopoeia. Meanwhile, the invention provides a detection method of the impurity I, and the impurity I and the content of the impurity I can be accurately and effectively detected from alogliptin benzoate. The preparation process is simple, stable and good in repeatability, the reference substance of the impurity I in the alogliptin benzoate can be prepared, the reference substance is used for quality control of the alogliptin benzoate, and the application prospect is good.

Description

technical field [0001] The invention belongs to the field of medicine quality control, and in particular relates to an alogliptin benzoate impurity, a preparation method and a detection method thereof. Background technique [0002] Alogliptin benzoate (Alogliptin benzoate) is a serine protease dipeptidyl peptidase Ⅳ (DPP-Ⅳ) inhibitor developed by Japan Takeda Company, which can maintain glucagon-like peptide 1 (GLP-1) in vivo And the level of glucose-dependent insulinotropic polypeptide (GIP), promote the secretion of insulin, thereby play a hypoglycemic effect. In April 2010, alogliptin benzoate was approved in Japan for the treatment of type 2 diabetes, under the trade name Nesina. In 2013, it was approved to enter the Chinese market with the product name "Nesina". [0003] Alogliptin benzoate is well tolerated by patients with type 2 diabetes mellitus, without dose-limiting toxicity, drug accumulation does not occur when multiple doses are administered, and patients wit...

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
IPC IPC(8): C07D239/553G01N30/04G01N30/02
CPCC07D239/553G01N30/04G01N30/02G01N2030/047G01N2030/027
Inventor 张菊华刘正超戴志东肖萍王婷
Owner 成都伊诺达博医药科技有限公司
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