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

Trospium chloride synthesis process

A technology of trospium chloride and a synthesis process, which is applied in the field of medicine and achieves the effects of low production cost, reduced pollution and high yield

Active Publication Date: 2012-10-10
SHOUGUANG FUKANG PHARMA +1
View PDF7 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the invention is to provide a kind of trospium chloride synthetic technique, to solve the deficiencies in the existing technique

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: the concrete steps of a kind of trospium chloride synthetic technique of the present invention are as follows:

[0029] ①Preparation of diphenylglycol chloride: Add 50g of diphenylglycolic acid and 130g of thionyl chloride into the reaction flask, reflux for 5 hours, and recover unreacted SOCl under reduced pressure 2 , and then add n-hexane for recrystallization to obtain 49 g of diphenylglycolyl chloride, yield 93%;

[0030] ② Preparation of nortropine alcohol: In an autoclave, add 100 g of α-tropine alcohol, dissolve in 500 mL of methanol, add 1 g of 10% Pd / C, 50 g of hydrochloric acid, replace with nitrogen, then pass hydrogen to 1 atm, and heat up to 60 ℃, heat preservation reaction for 2 hours, lowered to room temperature, filtered out the catalyst after pressure relief, and evaporated the solvent under reduced pressure to obtain 33 g of nortropine alcohol, with a yield of 73%;

[0031] ③Preparation of (3α-nortropine alcohol)-8-spiro-1-pyrrole ammon...

Embodiment 2

[0033] Embodiment 2: the concrete steps of a kind of trospium chloride synthetic technique of the present invention are as follows:

[0034] ①Preparation of diphenylglycol chloride: Add 50g of diphenylglycolic acid and 150g mL of thionyl chloride into the reaction flask, reflux for 5 hours, and recover unreacted SOCl under reduced pressure 2 , and then add n-hexane for recrystallization to obtain 50 g of diphenylglycolyl chloride, with a yield of 93%;

[0035] ② Preparation of nortropine alcohol: In an autoclave, add 100 g of α-tropine alcohol, dissolve in 500 mL of methanol, add 1.5 g of 10% Pd / C, 50 g of hydrochloric acid, replace with nitrogen, then pass hydrogen to 1 atm, and heat up to 60°C, heat preservation reaction for 2 hours, lower to room temperature, filter out the catalyst after pressure relief, and evaporate the solvent to dryness under reduced pressure to obtain 30 g of nortropine alcohol, with a yield of about 66%;

[0036] ③ Preparation of (3α-nortropine alco...

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 trospium chloride synthesis process which includes the steps: firstly, preparing benziloyl chloride; secondly, preparing nortropine; thirdly, preparing chloridized (3alpha-nortropine)-8-whorl-1-pyrrole ammonium salt; and fourthly, preparing the trospium chloride by condensing the benziloyl chloride and the chloridized (3alpha-nortropine)-8-whorl-1-pyrrole ammonium salt to obtain the trospium chloride. The trospium chloride synthesis process has the advantages that the reaction steps are short, atom economy is high, yield is high, production cost is low, catalysts can be repeatedly applied mechanically by a method for removing methyl through Pd / C catalytic hydrogenation, consumption of the catalysts is reduced, pollution is decreased, and complicated post-reaction treatment and the like are omitted.

Description

technical field [0001] The invention relates to medicines and is a synthesis process of trospium chloride. Background technique [0002] The chemical name of trospium chloride is -3-diphenylglycolyl nortropane-8-spiro-1-pyrrolidine chloride, which is mainly used to treat various detrusor muscle instability or detrusor hyperfunction. Frequent urination, urgency and urinary incontinence drugs, trospium chloride synthesis process currently mainly has two categories: one is: diphenylglycolic acid is activated with N,N-carbonyldiimidazole to prepare the intermediate diphenylglycoimidazole, to Metropine alcohol uses acetyl to protect the N atom, reacts with the intermediate diphenylglycol imidazole to form an ester, then deprotects it, and finally reacts with 1,4-dichlorobutane to prepare trospium chloride. [0003] . [0004] The other type is: diphenylglycol...

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): C07D451/00
CPCY02P20/584
Inventor 宋伟国董良军甲宗青夏艳田梅
Owner SHOUGUANG FUKANG 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