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Preparation method of D/L-dibenzoyl tartaric acid

A technology of benzoyl tartaric acid and tartaric acid, which is applied in the preparation of carboxylic acid salts, carboxylic acid esters, organic compounds, etc., can solve the problems of environmental pollution and high production costs, and achieve reduced production costs, convenient operation, and shortened process The effect of the process

Pending Publication Date: 2019-09-20
ZHEJIANG JIAHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, a large amount of benzoic acid by-products can be produced in the synthetic process of D / L-dibenzoyltartaric acid, resulting in the purity of the finished product being usually less than 98.5%, the product yield can only reach 76%, and the production cost per ton of product is relatively high. High; and the generated benzoic acid by-products also need further recovery treatment, and in the current prior art, saline waste water will be produced in the process of benzoic acid by-products, which will pollute the environment, thereby failing to meet people's requirements

Method used

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  • Preparation method of D/L-dibenzoyl tartaric acid
  • Preparation method of D/L-dibenzoyl tartaric acid
  • Preparation method of D/L-dibenzoyl tartaric acid

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Embodiment 1

[0027] A kind of preparation method of D / L-dibenzoyl tartaric acid, comprises the steps:

[0028] Step 1, get D / L-tartaric acid 100g, toluene 150mL and put into reactor, under the condition that stirring speed is 1000r / min, add 3g ferric chloride and 80g benzoyl chloride in reactor, stir After reacting for 20 minutes under the conditions of the reaction kettle, add 60 mL of trichlorobenzyl to the reaction kettle, and then continue to react for 60 minutes after adding; Continue to react for 45 minutes after ℃ to obtain the product mixture;

[0029] Step 2. After the product mixture obtained in step 1 is cooled to room temperature, it is transferred to a centrifuge at a speed of 600 r / min for centrifugation to finally obtain solid D / L-dibenzoyl tartaric acid.

Embodiment 2

[0031] A kind of preparation method of D / L-dibenzoyl tartaric acid, comprises the steps:

[0032] Step 1, get D / L-tartaric acid 100g, toluene 200mL and put into reactor, under the condition that stirring speed is 2500r / min, add the ferric chloride of 6g and the benzoyl chloride of 100g in reactor, stir After reacting for 40 minutes under the conditions of the reaction kettle, add 90 mL of trichlorobenzyl to the reaction kettle, and then continue to react for 50 minutes after adding; Continue to react for 30 minutes after ℃ to obtain the product mixture;

[0033] Step 2. After the product mixture obtained in step 1 is cooled to room temperature, it is transferred to a centrifuge at a speed of 900 r / min for centrifugation to finally obtain solid D / L-dibenzoyl tartaric acid.

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Abstract

The invention discloses a preparation method of D / L-dibenzoyl tartaric acid. The preparation method comprises following steps: step one, adding 100 parts of D / L-tartaric acid and a proper amount of a solvent into a reactor, then adding 2 to 10 parts of a catalyst and 80 to 110 parts of benzoyl chloride under stirring, carrying out reactions for 20 to 40 minutes under stirring, then adding 50 to 90 parts of benzenyl trichloride into the reactor, after addition, carrying out reactions for 45 to 60 minutes; then adding 100 to 200 parts of deionized water into the reactor, heating the materials in the reactor to a temperature of 90 to 100 DEG C, and carrying out reactions for 30 to 45 minutes to obtain a mixture (product); and step two, cooling the mixture to the room temperature, and transferring the mixture to a centrifuge to carry out centrifugal separation to obtain a solid namely D / L-dibenzoyl tartaric acid. The preparation method can largely improve the yield and reduces the production cost, generation of byproducts, and environmental pollution.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of D / L-dibenzoyltartaric acid. Background technique [0002] D / L-dibenzoyl tartaric acid is a white crystalline powder with low price, stable properties and easy recycling. It is widely used as an intermediate of levamisole and chiral resolution amine compounds. It has good properties Industrial application value. [0003] In the prior art, a large amount of benzoic acid by-products can be produced in the synthetic process of D / L-dibenzoyltartaric acid, resulting in the purity of the finished product being usually less than 98.5%, the product yield can only reach 76%, and the production cost per ton of product is relatively high. High; and the generated benzoic acid by-products also need further recovery treatment, and in the current prior art, saline waste water will be produced in the process of benzoic acid by-products, which will pollute the e...

Claims

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Application Information

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IPC IPC(8): C07D307/62C07C67/29C07C69/78C07C51/60C07C63/10
CPCC07D307/62C07C67/29C07C51/60C07C69/78C07C63/10
Inventor 周少华林世清何贺龙胡菁江晓飞
Owner ZHEJIANG JIAHUA CHEM
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