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Synthesis method of D-dibenzoyl tartaric acid

A technology of dibenzoyl tartaric acid and dibenzoyl tartaric anhydride is applied in the field of chemical synthesis of chiral resolution reagents, which can solve the problems of low utilization rate of raw materials, inability to recycle, large production pollution, etc., and achieve convenient operation, The effect of low cost, improved product yield and product quality

Inactive Publication Date: 2015-04-22
濮阳天健生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The defect of common synthetic method is: 1. raw material has strong irritation, strong corrosiveness, hypertoxicity, is difficult to handle
② The utilization rate of raw materials is low, they cannot be recycled, and the production pollution is relatively large
③ The process yield is low, about 40%, the product purity is low, and the production cost is high

Method used

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  • Synthesis method of D-dibenzoyl tartaric acid
  • Synthesis method of D-dibenzoyl tartaric acid
  • Synthesis method of D-dibenzoyl tartaric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of synthetic method of D-dibenzoyl tartaric acid, it comprises the steps: take D-tartaric acid 150g, toluene 200ml and place 1000ml there-necked bottle, add 1g of copper sulfate under stirring, begin to drop 300g of benzoyl chloride, drip in 2 hours Finished, continue to react for 4 hours, put the material into the centrifuge, and get 438.7g of D-dibenzoyl tartaric anhydride by shaking filter, put it into a 2000ml three-necked bottle, add 438.7g of water and toluene, heat up to reflux, keep for 3 hours, cool down The material was discharged at room temperature, and 344.1 g of D-dibenzoyl tartaric acid was obtained by rejection filtration.

[0036] The D-dibenzoyl tartaric acid that present embodiment obtains is carried out TEM test, test structure such as figure 1 Shown, as can be seen from the figure, the finished product D-dibenzoyl tartaric acid purity content is 99.20%, and the total yield is 95.3%.

[0037] Peak number Peak name Retention time Peak height P...

Embodiment 2

[0052] A kind of synthetic method of D-dibenzoyl tartaric acid, it comprises the steps:

[0053] Put 1.5kg of D-tartaric acid and 2L of toluene into a 10L three-necked bottle, add 11g of copper sulfate under stirring, start to add 3.8kg of benzoyl chloride dropwise, finish dropping in 2.5 hours, continue to react for 4 hours, discharge the material into a centrifuge, and shake off to obtain D-dibenzoyl tartaric anhydride 4.32kg, put it into a 20L three-necked bottle, add water and toluene each 4.32kg, heat up to reflux, keep for 3 hours, cool to normal temperature and discharge, shake off to get D-dibenzoyl tartaric acid 3.45kg kg.

[0054] The D-dibenzoyl tartaric acid that present embodiment obtains is carried out TEM test, test structure such as figure 2 Shown, as can be seen from the figure, the finished product D-dibenzoyl tartaric acid purity content is 99.38%, and the total yield is 95.8%.

[0055] Peak number Peak name Retention time Peak height Peak area Content

...

Embodiment 3

[0069] A kind of synthetic method of D-dibenzoyl tartaric acid, it comprises the steps:

[0070] Put 7.5kg of D-tartaric acid and 10L of toluene into a 50L reactor, add 45g of ferrous sulfate under stirring, start to add 18kg of benzoyl chloride dropwise, finish dripping in 3.5 hours, continue to react for 4 hours, discharge the material to a centrifuge, and shake off to obtain D-dibenzoyl tartaric anhydride 20.7kg, put it into a 100L reactor, add water and toluene each 20.7kg, heat up to reflux, keep for 3 hours, cool down to normal temperature and discharge, shake off to get D-dibenzoyl tartaric acid 17.1 kg.

[0071] The D-dibenzoyl tartaric acid that present embodiment obtains is carried out TEM test, test structure such as image 3 Shown, as can be seen from the figure, the finished product D-dibenzoyl tartaric acid purity content is 99.05%, and the total yield is 95.5%.

[0072] Peak number Peak name Retention time Peak height Peak area Content

[0073] 1 2.455 266.13...

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Abstract

The invention relates to a synthesis method of D-dibenzoyl tartaric acid. The synthesis method comprises the following steps: reacting by taking D-tartaric acid and benzoyl chloride as raw materials, taking copper sulfate as a catalyst and taking toluene as a solvent to prepare D-dibenzoyl tartaric acid anhydride, adding an equal amount of water, and performing hydrolysis with toluene to obtain D-dibenzoyl tartaric acid, wherein the solvent, namely toluene, and the water and toluene in the hydrolysis step can be recycled. The method provided by the invention has the advantages of simple process, safety, easiness in operation and high process yield of above 95%; and simultaneously, the cost of the raw materials is relatively low, part of the raw materials can be recycled, the purity of a finished product is relatively high, and the chiral separation performance is excellent.

Description

technical field [0001] The invention relates to the technical field of a chemical synthesis method of a chiral resolution reagent, in particular to a synthesis method of D-dibenzoyltartaric acid. Background technique [0002] D-Dibenzoyltartaric acid is a white crystalline powder. It is widely used as an intermediate of the anthelmintic drug levamisole and chiral resolution of amine compounds. And because of its low price, stable properties, and easy recycling, it has good industrial application value. Its molecular formula is as follows: [0003] [0004] The defect of common synthetic method is: 1. raw material has strong irritation, strong corrosiveness, hypertoxicity, is difficult for handling. ② The utilization rate of raw materials is low, they cannot be recycled, and the production pollution is relatively large. ③The process yield is low, about 40%, the product purity is lower, and the production cost is higher. Contents of the invention [0005] The technic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/78C07C67/297
CPCC07C67/297C07D307/60C07C69/78
Inventor 崔清海李志军楚静波刘航张道伟崔飞李亚敏王建勋李荣范卫彬郑记栓袁国龙文教刚张建民
Owner 濮阳天健生物科技有限公司
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