Asymmetric diphenic acid isomeride separation method

A technology of isomers and diphenylformic acid, which is applied in the field of separation of asymmetric biphenylformic acid isomers, can solve the problems of cumbersome operation, long encapsulation time, general separation effect, etc., and achieve mild reaction conditions, Easy to operate and good separation effect

Inactive Publication Date: 2015-11-11
启东东岳药业有限公司 +1
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] When 2-methyl-9-fluorenone is prepared by ring-opening under the condition of potassium tert-butoxide to prepare I, asymmetric ring-opening occurs, and the proportion of ring-opening product I is 60%, and the proportion of ring-opening product II is 40%. The properties of the two products are very similar, and it is difficult to achieve separation to obtain the target product Ⅰ
[0005] For the separation of isomers with dibenzoic acid structure, the following methods are mainly included: one is to use the different

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
  • Asymmetric diphenic acid isomeride separation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put the mixed acid (4.24g, 20mmol) and potassium hydroxide (1.12g, 20mmol) in a reaction flask, add 100mL of water, stir it magnetically to dissolve it, then heat it in an oil bath, and distill part of the water to make the solution slightly cloudy , and then cooled to 0°C, a white solid was precipitated, filtered, the filter cake was redissolved in water, and hydrochloric acid was added to adjust the pH to 4-6, the solid was precipitated, filtered, and dried to obtain 1.42g of product, the yield was 33.5%, Ⅰ The purity is 76%.

Embodiment 2

[0026] Put mixed acid (4.24g, 20mmol) and calcium hydroxide (0.74g, 10mmol) in a reaction flask, add 100mL of water, stir magnetically and add an oil bath to make it dissolve, continue to heat up to distill part of the water to make the solution slightly It was turbid, then cooled to 0°C, a white solid was precipitated, filtered, the filter cake was redissolved in water, and hydrochloric acid was added to adjust the pH to 4-6, the solid was precipitated, filtered, and dried to obtain 1.61g of product with a yield of 38.0%. I has a purity of 87%.

Embodiment 3

[0028] Put the mixed acid (6.36g, 30mmol) and aluminum hydroxide (0.78g, 10mmol) in a reaction flask, add 200mL of water, stir magnetically and add an oil bath to make it dissolve, continue to heat up and distill part of the water to make the solution slightly It was turbid, then cooled to 0°C, a white solid was precipitated, filtered, the filter cake was redissolved in water, and the pH was adjusted to 4-6 by adding hydrochloric acid, the solid was precipitated, filtered, and dried to obtain 3.31 g of the product, with a yield of 52.0%. I has a purity of 72%.

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 discloses an asymmetric diphenic acid isomeride separation method, which includes the steps of mixing mixed acid and inorganic alkali in a water solution, stirring the solution to clarify the solution to obtain metal salt, performing heating reflux to distill partial water out to turbid the solution, cooling the solution to precipitate-out solid, re-dissolving the solid in the water solution, and performing acidification to obtain the product. The method is mild in reaction conditions, is simple in operation and is good in separation effect.

Description

technical field [0001] The invention relates to a method for separating isomers of unsymmetrical dibenzoic acid. Background technique [0002] 4'-Methyl-[1,1'-biphenyl]-2-carboxylic acid (I) is often used as an intermediate in organic synthesis and can be used to synthesize sartan biphenyl. [0003] When 2-methyl-9-fluorenone is prepared by ring-opening under the condition of potassium tert-butoxide to prepare I, asymmetric ring-opening occurs, and the proportion of ring-opening product I is 60%, and the proportion of ring-opening product II is 40%. The properties of the two products are very close, and it is difficult to achieve the separation to obtain the target product I. Its ring-opening reaction equation is as follows: [0004] [0005] For the separation of isomers with dibenzoic acid structure, the following methods are mainly included: one is to use the different acidity of the mixture to separate, but the acidity of such isomers is mostly similar, and it is di...

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
IPC IPC(8): C07C51/487C07C63/331
CPCC07C51/487C07C63/331
Inventor 王巧纯龙中柱安娜汪家宏刘建森金伟群
Owner 启东东岳药业有限公司
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