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Preparation method of (-)-di(p-toluoyl)tartaric acid

A technology of toluoyl tartaric acid and p-toluic acid, which is applied in the field of preparation of optical acid resolving agents, can solve the problems of many production links, cumbersome production steps, difficulty in meeting the needs of scientific research and production, and achieve the effect of simple process

Inactive Publication Date: 2010-06-02
南通欧通置业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In scientific research and actual production, the commonly used optical acid resolving agents are very limited, only limited to a few such as tartaric acid, which is difficult to meet the needs of scientific research and production. It is very urgent to develop new varieties of optical acid resolving agents
(-)-Di-p-toluoyl tartaric acid is a kind of tartaric acid resolving agent. At present, the synthesis method has been reported, but the production steps are relatively cumbersome, and there are many production links, which affect the production efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A, the preparation of p-toluoyl chloride:

[0021] In a 500ml flask equipped with a reflux condenser, add 100g of p-toluic acid, 200g of toluene and 2g of DMF, and simultaneously add 120g of thionyl chloride dropwise. After the dropwise addition is complete, heat to reflux for 4 hours.

[0022] B, the preparation of (-)-two p-toluoyl tartaric acid:

[0023] Add 65g tartaric acid in above-mentioned reaction liquid, heat reflux 2 hours. After the reaction is finished, cool down to room temperature and adjust to neutrality with liquid caustic soda. After the pH adjustment is completed, heat and reflux for 3 hours. After the reaction is complete, discharge the material while it is hot, cool to below 20° C., filter out the crystals, wash twice with the reaction solvent, and dry to obtain 241 g of white crystals with a yield of 85%.

Embodiment 2

[0025] A, the preparation of p-toluoyl chloride:

[0026] In a 500ml flask equipped with a reflux condenser, add 100g of p-toluene, 300g of toluene and 4g of DMF, and simultaneously add 140g of thionyl chloride dropwise, and heat to reflux for 6 hours after the dropwise addition is complete.

[0027] B, the preparation of (-)-two p-toluoyl tartaric acid:

[0028] Add 70g of tartaric acid in above-mentioned reaction liquid, heat and reflux for 4 hours. After the reaction is finished, cool down to room temperature and adjust to neutrality with liquid caustic soda. After the pH adjustment is completed, heat and reflux for 1 hour. After the reaction is complete, discharge the material while it is hot, cool to below 20° C., filter out the crystals, wash twice with the reaction solvent, and dry to obtain 250 g of white crystals with a yield of 87%.

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Abstract

The invention discloses a preparation method of (-)-di(p-toluoyl)tartaric acid. The preparation method comprises the following steps of: adding certain quantity of para-toluylicacid, solvent and catalyst into a flask which is provided with a reflux condenser, simultaneously dropwise adding thionyl chloride; and then adding certain quantity of tartaric acid after heating for reflux for a while; then continuing to heat for reflux for a while; after reaction is finished, cooling to room temperature; adjusting pH value to be neutral by using an alkali solution; after finishing pH adjusting, heating for reflux for a while; after reaction, cooling to below 20 DEG C; filtrating to obtain a crystal; washing twice with a reactive solvent; and baking to obtain the product. The process has the characteristics of simple process, high efficiency, direct product obtaining without treating a semi-finished product, and adaptability to actual production.

Description

technical field [0001] The invention relates to a preparation method of an optical acid resolving agent, in particular to a preparation method of (-)-di-p-toluoyl tartaric acid. Background technique [0002] In scientific research and actual production, the commonly used optical acid resolving agents are very limited, only limited to a few such as tartaric acid, which is difficult to meet the needs of scientific research and production. It is very urgent to develop new varieties of optical acid resolving agents. (-)-Di-p-toluoyl tartaric acid belongs to a kind of tartaric acid resolving agent. At present, the synthesis method has been reported, but the production steps are relatively cumbersome, and there are many production links, which affect the production efficiency. Contents of the invention [0003] The purpose of the present invention is to provide a kind of preparation method of (-)-di-p-toluoyl tartaric acid with simple process and adapting to actual production ne...

Claims

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Application Information

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IPC IPC(8): C07C69/76C07C67/14
Inventor 周成云
Owner 南通欧通置业有限公司
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