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Method for preparing monophenyl maleate derivative under condition of no solvent

A technology of monophenyl maleate and monophenyl maleate, applied in the field of preparation of monophenyl maleate derivatives, achieving high yield, simple post-processing, and convenient and easy raw materials The effect

Inactive Publication Date: 2010-09-22
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Before the present invention was made, there was no bibliographical report on the preparation method of 6-substituted-4-chromanone-2-carboxylic acid and its derivatives under solvent-free and homogeneous base catalyst

Method used

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  • Method for preparing monophenyl maleate derivative under condition of no solvent
  • Method for preparing monophenyl maleate derivative under condition of no solvent
  • Method for preparing monophenyl maleate derivative under condition of no solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0015] The preparation of embodiment 1~3 monophenyl maleate

[0016] Take 0.94g (10mmol) phenol and 0.98g (10mmol) maleic anhydride in a mortar, add 1.06g (10mmol) Na under grinding at room temperature 2 CO 3 Solid base catalyst, continue grinding and stirring for 5min. After the reaction was completed, hydrochloric acid with a concentration of 10%±0.01 was added until white crystals were no longer precipitated. Suction filtration, washing with water, drying, and purification by column chromatography yielded 1.052 g of monophenyl maleate with a yield of 54.79%. The reaction temperature was 119-120° C. and the purity was 98.6%.

[0017] Under the constant situation of the amount of feeding material, use different solid base catalysts to catalyze the reaction, its operation is the same as above, wherein the solid base catalyst is shown in Table 1, and the test results are shown in Table 1:

[0018] Table 1 test embodiment 1~3 test result

[0019]

Embodiment 4～8

[0020] The preparation of embodiment 4~8 maleic acid monophenyl ester

[0021] 10mmol of phenol, 10mmol of maleic anhydride, solid Na 2 CO 3 The catalyst consumption is shown in Table 2, and the reaction is carried out at room temperature, and other operations are the same as in Example 1. The test results are shown in Table 2:

[0022] Table 2 test embodiment 4~8 test result

[0023]

Embodiment 9～13

[0024] The preparation of embodiment 9~13 monophenyl maleate

[0025] 10mmol of phenol, 10mmol of maleic anhydride, solid Na 2 CO 3 10mmol, the reaction time is shown in Table 3, the reaction is carried out at room temperature, and other operations are the same as in Example 1. The test results are shown in Table 3:

[0026] Table 3 test embodiment 9~13 test result

[0027]

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Abstract

The invention relates to a method for preparing a monophenyl maleate derivative under the condition of no solvent. The monophenyl maleate derivative is an important intermediate in the preparation of 6-substituted-4-chromanone-2-formic acid having wide physiological activities and pharmaceutical activities and a derivative thereof and widely used in the fields of medicines, agrochemicals, the organic synthesis of intermediates and the like. The invention provides a method for preparing the monophenyl maleate derivative by a solvent-free synthesis method. The method adopts the technical schemethat under the condition of no solvent, a phenol compound serves as a raw material reacts with maleic anhydride under the catalysis of a solid base to generate the monophenyl maleate derivative with the reaction yield of 35.9 to 69.8 percent. The method of the invention has the advantages of cheap and available catalyst, mild reaction condition, simple and safe operation, simple post-treatment and the like, particularly has greater environmental protection significance and social and economic benefits under the condition of no solvent.

Description

technical field [0001] The invention relates to a preparation method of maleic acid monophenyl ester derivatives without solvent. Background technique [0002] Maleic acid monophenyl ester derivatives are important intermediates for the synthesis of 6-substituted-4-chromanone-2-carboxylic acid and its derivatives, 6-substituted-4-chromanone-2-carboxylic acid derivatives The good physiological and pharmacological activities of the compound have been paid attention to by people, and its derivatives have been found to have good physiological activities such as promoting development, desensitization and antifungal, and have anticancer activity. [0003] Before the present invention was made, there was no literature report on the preparation method of 6-substituted-4-chromanone-2-carboxylic acid and its derivatives under solvent-free and homogeneous base catalyst. [0004] The invention conforms to the idea of ​​green chemistry. One of the most important goals of "green" chemis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B41/12C07C67/08C07C69/60C07C69/657C07C201/12C07C205/43
Inventor 柏一慧杨林芳
Owner ZHEJIANG NORMAL UNIVERSITY