Method for salifying or recrystallization of rupatadine fumarate

A technology of rupatadine fumarate and fumaric acid, which is applied in the field of salt formation or recrystallization of anti-allergic drugs, can solve the problems of being unsuitable for large-scale industrial production, affecting product quality and yield, and low solubility. Achieve good crystal stability and fluidity or bulk density, good quality, and good solubility

Inactive Publication Date: 2011-04-27
NANJING VARSAL MEDICINE TECH DEV +1
View PDF3 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Based on the high residual capacity requirements of methanol, and it is a second-class solvent, it is more toxic; ethyl acetate and ethanol have low solubility to fumaric acid and rupatadine, which affects product quality and yield, and is not suitable for large-scale industrialization Production and other reasons; the existing technology is prone to encapsulation of fumaric acid or rupatadine

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
  • Method for salifying or recrystallization of rupatadine fumarate
  • Method for salifying or recrystallization of rupatadine fumarate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 16 grams of free base rupatadine and 320ml of the solution (acetone:water=9:1, volume ratio) into a 500ml three-necked flask, turn on mechanical stirring, heat up to 40°C, and add 4.48 grams of fumaric acid, after the addition, stir at 40°C for 30 minutes, then cool to about 0°C and stir to crystallize overnight, filter, wash the solid with cold acetone, and dry in vacuum at 60-70°C for 8 hours to obtain 17.5 grams of fumaric acid The white powder of patadine has a yield of 85.4%.

[0021] By the X-ray diffraction method, the product obtained in the embodiment is placed on a powder diffractometer for scanning and X-ray radiation, and the measured results are expressed at about 8.0 (10.8), about 11.6 (7.46), about 12.5 (7.02), There are characteristic peaks at about 13.7 (6.42), about 16.8 (5.28), about 19.6 (4.5), about 20.2 (4.35), and about 24.3 (3.63). Such as figure 1 shown.

[0022] Check the infrared absorption spectrum of the product with a spectrophotomet...

Embodiment 2

[0025] Add 16 grams of free base rupatadine and 320 ml of the solution (acetone: water = 5: 1, volume ratio) into a 500 ml three-necked flask, turn on mechanical stirring, raise the temperature to 40 ° C, and add 4.48 grams of fumaric acid, after the addition, stir at 40°C for 30 minutes, then cool to about 0°C and stir to crystallize overnight, filter, wash the solid with cold acetone, and dry in vacuum at 60-70°C for 8 hours to obtain 16.4 grams of fumaric acid The white powder of patadine has a yield of 80.1%.

Embodiment 3

[0027] Add 16 grams of free base rupatadine and 320 ml of the solution (acetone: water = 15: 1, volume ratio) into a 500 ml three-necked flask, turn on mechanical stirring, heat up to 40 ° C, and add 4.48 grams of fumaric acid, after the addition, stir at 40°C for 30 minutes, then cool to about 0°C and stir to crystallize overnight, filter, wash the solid with cold acetone, and dry in vacuum at 60-70°C for 8 hours to obtain 17.6 grams of fumaric acid The white powder of patadine has a yield of 86.0%.

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 method for preparing rupatadine fumarate, which is suitable for actual large-scale industrial production and has high yield and quality and excellent stability. A preparation method for the salifying of the rupatadine fumarate comprises the following step of performing a salifying reaction on rupatadine and fumaric acid in a mixed solvent, wherein the mixed solvent is a mixed solvent of acetone and water in a volume ratio of 5-20:1. In addition, the rupatadine fumarate also can be subjected to recrystallization in the mixed solvent.

Description

technical field [0001] The invention relates to a salt-forming or recrystallization method of an antiallergic drug, in particular to a salt-formation or recrystallization method of rupatadine fumarate. Background technique [0002] The chemical name of rupatadine fumarate is 8-chloro-11-[1-[(5-methyl-3-pyridyl)methyl]piperidin-4-ylidene]-6,11 - Dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine (E)-2-butenedioate. It is an antiallergic drug with dual effects of antagonizing histamine and platelet activating factor, suitable for treating diseases such as perennial allergic rhinitis and hay fever, and is currently widely used in clinical use. In order to obtain raw materials of rupatadine fumarate with higher quality and more suitable for application, technical personnel have improved its preparation process. [0003] In 1993, ES2087818 disclosed the use of a single solvent, ethanol, as a solvent for rupatadine fumarate salt formation and crystallization, but under this process ...

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 Applications(China)
IPC IPC(8): C07D401/14
Inventor 孙珏曾裕建叶祥黎鹏胡林郁经才周惠王金强
Owner NANJING VARSAL MEDICINE TECH DEV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap