Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing colesevelam hydrochloride by solution polymerization

A technology of colesevelam hydrochloride and polymerization reaction, which is applied in the field of drug synthesis, can solve the problems of not being simple and simple in operation steps and not easy to control the degree of crosslinking, and achieve the goal of easy control of grafting rate, guarantee of stability and high reproducibility Effect

Active Publication Date: 2017-11-14
XINFA PHARMA
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method needs to go through three steps of polymerization, hydrolysis and crosslinking. The operation steps are not simple enough and the degree of crosslinking is not easy to control.

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 preparing colesevelam hydrochloride by solution polymerization
  • Method for preparing colesevelam hydrochloride by solution polymerization
  • Method for preparing colesevelam hydrochloride by solution polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Preparation of monomer B (1,3-diallylamino-2-hydroxypropane)

[0035]

[0036] In a four-necked flask equipped with stirring, a thermometer, a constant pressure dropping funnel, and a condensing reflux tube, add 350 grams of 1,2-dichloroethane, 57.0 grams (1.0 moles) of allylamine, 79.0 grams (0.5 moles) ) Potassium carbonate, heated and kept at 40-45°C and slowly added 46.2 grams (0.5 moles) of epichlorohydrin dropwise, and the dropwise addition was completed in about 4 hours. 20-25°C, filter, wash the filter cake with 50 g of 1,2-dichloroethane, combine the organic phases, recover 1,2-dichloroethane by atmospheric distillation, and then distill under reduced pressure to obtain a colorless transparent liquid 1,3 - Diallylamino-2-hydroxypropane 80.3 g, GC purity 99.8%, yield 94.5%.

Embodiment 2

[0037] Example 2: Preparation of monomer B (1,3-diallylamino-2-hydroxypropane)

[0038] Replace the 1,2-dichloroethane in Example 1 with tetrahydrofuran of the same quality, and the rest are the same as in Example 1 to obtain 81.1 grams of colorless and transparent liquid 1,3-diallylamino-2-hydroxypropane, with a GC purity of 99.7%, the yield is 95.3%.

Embodiment 3

[0039] Embodiment 3: the preparation of monomer C (N-allyl n-decylamine)

[0040]

[0041] In a four-necked flask equipped with stirring, a thermometer, a constant pressure dropping funnel, and a condensing reflux tube, add 550 grams of 1,2-dichloroethane, 57.0 grams (1.0 moles) of allylamine, 138.0 grams (1.0 moles) ) Potassium carbonate, heated and kept at 40-45°C, and slowly added 221.0 grams (1.0 mole) of 1-bromodecane dropwise, and the dropwise addition was completed in about 4 hours, and continued to stir and react at 60-65°C for 6 hours, and cooled to 20-25°C, filter, wash the filter cake with 100 g of 1,2-dichloroethane, combine the organic phases, recover 1,2-dichloroethane by atmospheric distillation, and then distill under reduced pressure to obtain a colorless transparent liquid N-ene Propyl n-decylamine 190.5 g, GC purity 99.5%, yield 96.7%.

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 relates to a method for preparing colesevelam through solution polymerization. According to the method, in the presence of a solvent and an initiator, the monomer A allyl amine, the monomer B 1,3-diallyl amino-2-hydroxyl propane, the monomer C N-allyl decylamine and the monomer D 6-n-hexyl allyl amino trimethyl ammonium chloride are subjected to free radical polymerization and hydrochloric acid salifying to generate the colesevelam. The process is easy to operate, and the degree of polymerization and grafting ratio of the colesevelam can be easily controlled.

Description

technical field [0001] The invention relates to a preparation method of solution polymerization colesevelam hydrochloride, which belongs to the technical field of medicine synthesis. Background technique [0002] Colesevelam hydrochloride is a non-absorbable polymer lipid-lowering drug, suitable for the treatment of excessive serum total cholesterol (TC) or triglyceride (TG) levels. Used alone or in combination with a statin can reduce high levels of low-density lipoprotein cholesterol (LDL-C) in patients with primary hypercholesterolemia. Colesevelam Hydrochloride, a pro- Water-based insoluble light yellow powder polymer, its chemical structure is as shown in formula I: [0003] [0004] The synthetic route of colesevelam hydrochloride generally comprises the following steps at present: 1. prepare allylamine hydrochloride by allylamine; 2. allylamine hydrochloride carries out radical polymerization under free radical initiator, Form allylamine polymer; 3. The allylamin...

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): C08F226/02C08F226/04
CPCC08F226/02C08F226/04
Inventor 戚聿新马新娜李广乾王世明陈军
Owner XINFA PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com