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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
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  • 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 acidity of the mixture to separate, but the acidity of such isomers is mostly similar, and it is difficult to achieve a good separation effect; The second is to use the inclusion method for separation, mainly using β-cyclodextrin for inclusion separation. This method requires a long time for inclusion and separation, and the operation is relatively cumbersome; the third is to use different solubility in aqueous or organic solutions for separation, but this method Isomers with similar solubilities and moderate separation

Method used

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  • Asymmetric diphenic acid isomeride separation method

Examples

Experimental program
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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%.

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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

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Application Information

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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
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