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Preparation process of thiatro bromoaminium anhydrous compound

A technology of tiotropium bromide and anhydrate, which is applied in the field of preparation of tiotropium bromide anhydrate, and can solve problems such as the lack of tiotropium bromide anhydrate

Active Publication Date: 2008-08-13
HONGYI SCI & TECH CO LTD NANCHANG
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Search Chinese Patent Database (1985-2005), Chinese Science and Technology Periodical Database (1989-2005), Digital Periodical Full-text Database (Wanfang) (1997-2005), Chinese Periodical Full-text Database (Tsinghua Tongfang) via internet search (1993-2005), National Science and Technology Achievement Transaction Database (1987-2005), China Applicable Technology Achievement Database (2005 Edition), Chinese Academic Conference Papers Database (1991-2005), National Science and Technology Achievement Database (1990 2005), China Science and Technology Economic News Database (1992-2005), PCT International Patent Application Database (1980-2005), European Patent Database (1980-2005), US Patent Database (1978-2005) 2005), U.S. Chemical Abstracts, etc., the results show that there is no report of making tiotropium bromide anhydrous as starting raw material with scopolamine hydrobromide

Method used

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  • Preparation process of thiatro bromoaminium anhydrous compound
  • Preparation process of thiatro bromoaminium anhydrous compound
  • Preparation process of thiatro bromoaminium anhydrous compound

Examples

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Embodiment Construction

[0004] 1. Preparation of Scopolamine (Intermediate 1)

[0005] Take scopolamine hydrobromide, add methanol and potassium carbonate, heat and stir, evaporate to dryness under reduced pressure, add dichloromethane, filter, wash the filter cake three times with dichloromethane, combine the filtrates, dry over anhydrous sodium sulfate, evaporate to dryness under reduced pressure, Obtain scopolamine oil (intermediate one), set aside.

[0006] 2. Preparation of bis(2-thienyl)glycolic acid methyl ester (intermediate 2)

[0007] Take bromothiophene and dissolve it in the ether solution dried by sodium, add dropwise to the ether solution dried by magnesium chips and sodium, after dropping, reflux and cool for later use.

[0008] Take a solution of dimethyl oxalate dissolved in ether, add it dropwise to the above Grignard solution, after dropping, reflux reaction, cool, add dilute sulfuric acid dropwise, separate the ether layer, wash with aqueous sodium carbonate solution, wash with w...

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Abstract

An anhydrous tiotropium bromide is prepared from scopolamine hydrobromate. Its preparing process is also disclosed.

Description

technical field [0001] The invention relates to a preparation method of tiotropium bromide anhydrate, which is characterized in that the tiotropium bromide anhydrate is synthesized by using scopolamine hydrobromide as a starting material. Background technique [0002] Tiotropium bromide (Tiotropium Bromide) was approved for listing in the Netherlands in November 2001 for the treatment of chronic obstructive pulmonary disease (COPD). Its basic patent is EP418716, which was proposed on September 12, 1990 by the German BoehringerIngelheim company , its invention name is "Thienylcarboxylic acid ester of aminoalcohols, their quaternary products, their preparation and use of the compounds", what the patent claims is tiotropium bromide monohydrate and its synthetic route with bromothiophene as the starting material and Uses for the treatment of COPD, etc. Search Chinese Patent Database (1985-2005), Chinese Science and Technology Periodical Database (1989-2005), Digital Periodical ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D451/00C07D491/18
Inventor 陶腾峰吕良忠许军钱进彭红李平刘孝乐
Owner HONGYI SCI & TECH CO LTD NANCHANG
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