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

Method for producing specific crystalline modifications of polymorphous substances

A crystal, a specific technology, applied in the fields of botanical equipment and methods, separation methods, crystallization bed crystallization, etc., can solve the problems of high processing cost and time-consuming development.

Inactive Publication Date: 2008-01-09
BAYER IP GMBH
View PDF9 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, typically specially designed additives must be specially synthesized to exert a specific influence on polymorphism, making their development time-consuming and the processing costs to employ them too high

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 producing specific crystalline modifications of polymorphous substances
  • Method for producing specific crystalline modifications of polymorphous substances

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0036] The stability of 2-(2-chloro-4-methylsulfonyl-benzoyl)cyclohexane-1,3-dione (sulcotrione) Preparation of a given crystal structure (modification II) by direct precipitation (additive: heterocyclic amine)

[0037] A toluene suspension of the triethylamine salt of 2-(2-chloro-4-methylsulfonyl-benzoyl)cyclohexane-1,3-dione, with the aid of the corresponding enol ester 3-oxo-cyclo Prepared by rearrangement of hex-1-enyl-(2-chloro-4-methanesulfonylbenzoate) (see EP-A2-186 117). The enol ester is here obtained by reacting 0.2 mol of 2-chloro-4-methanesulfonyl-benzoyl chloride with an equimolar amount of cyclohexane-1,3-dione in toluene in the presence of an excess of triethylamine as base synthesized by coupling. This toluene suspension was contacted with 500 g of dilute sodium hydroxide (4% by weight) at 45° C. for 30 min in order to obtain, as product, the sodium salt dissolved in the aqueous phase and free of by-products. After phase separation, the aqueous sodium en...

example 2

[0041] The stability of 2-(2-chloro-4-methylsulfonyl-benzoyl)cyclohexane-1,3-dione (sulcotrione) Preparation of a given crystal structure (modification II) by direct precipitation (additive: ketone)

[0042] The procedure described in Example 1 was carried out in an analogous manner but with a ketone as an additive in order to obtain 2-(2-chloro-4-methanesulfonyl-benzoyl)cyclohexane-1 directly by precipitation crystallization from the corresponding aqueous solution of sodium enolate, Stable crystal structure of 3-diketone (modification II). The crystal structure thus obtained was determined to be characterized by the characteristic Raman spectrum given in Example 1. The results of the ketones used, amounts and methods are shown in Table I.

[0043] Table I

[0044] example

example 3

[0046] The stability of 2-(2-chloro-4-methylsulfonyl-benzoyl)cyclohexane-1,3-dione (sulcotrione) Preparation of a given crystal structure (modification II) by direct precipitation (additive: alcohol)

[0047] The procedure described in Example 1 was carried out in a similar manner but with various alcohols as additives in order to obtain 2-(2-chloro-4-methanesulfonyl-benzoyl)cyclohexane directly by precipitation crystallization of the corresponding aqueous sodium enolate solution- Stable crystal structure of a 1,3-diketone (modification II). The crystal structure thus obtained was determined to be characterized by the characteristic Raman spectrum given in Example 1. The results of the alcohols used, amounts and methods are given in Table II.

[0048] Table II

[0049] example

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 concerns a method for producing specific crystalline modifications of an organic polymorphous substance. In accordance with said method, the specific crystalline modification is obtained by precipitation from a salt of the polymorphous substance present in an aqueous solution, by means of standard water-soluble organic solvents used as additives and an acid or a base.

Description

technical field [0001] The present invention relates to a method for producing polymorphs, specific crystal modifications of organic substances, by precipitating specific crystal modifications from aqueous solutions of salts of polymorphic substances using common water-soluble organic solvents as additives and acids or bases. Background technique [0002] Polymorphism of active substances is important for chemical research, process development and formulation development. It is known that certain organic substances exist in only one crystal structure, while others (referred to as polymorphs) exist in two or more structures (referred to as modifications or crystal variants). It is not possible to predict the number of crystal variants, including their physicochemical properties, especially their thermodynamic stability, and their different behavior when administered to living organisms. [0003] It is known that for some polymorphs a particular variant represents a thermodyn...

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): B01D9/00C07C317/46A01N41/10B01D9/02C07C317/24C07C319/28C07C323/22
CPCB01D9/0036A01N41/10C07C2101/14C07C317/24C07C2601/14
Inventor A·埃布勒W·西尔格斯U·施维多普A·海恩
Owner BAYER IP GMBH
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