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A kind of synthetic method of d-p-methyldibenzoyl tartaric acid

A technology of methyl dibenzoyl tartaric acid and methyl dibenzoyl tartaric anhydride, applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of carboxylic acid halides, etc., can solve the problem of low raw material utilization rate and non-recyclable Utilization, low product purity and other problems to achieve the effects of convenient operation, low cost, and improved product yield and product quality

Active Publication Date: 2016-04-20
濮阳天健生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 35%, the product purity is low, and the production cost is high

Method used

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  • A kind of synthetic method of d-p-methyldibenzoyl tartaric acid
  • A kind of synthetic method of d-p-methyldibenzoyl tartaric acid
  • A kind of synthetic method of d-p-methyldibenzoyl tartaric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of synthetic method of D-p-methyl dibenzoyl tartaric acid, it comprises the steps:

[0036] Take 150g of D-tartaric acid and 200ml of toluene in a 1000ml three-neck bottle, add 1.5g of copper sulfate under stirring, start to add 330g of p-toluoyl chloride dropwise, finish dropping in 3 hours, continue to react for 6 hours, discharge the material into a centrifuge, and shake Filter to get 495.4g of D-p-methyldibenzoyl tartaric anhydride, put it into a 2000ml three-necked bottle, add 495.4g of water and toluene, heat up to reflux, keep it for 5 hours, cool down to normal temperature and discharge, shake off to get D-p Methyl dibenzoyl tartaric acid 374.4g.

[0037] The D-p-methyldibenzoyl 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-p-methyldibenzoyl tartaric acid purity content is 99.61%, and the total yield is 96.6%.

[0038] Peak Number Peak ...

Embodiment 2

[0049] A kind of synthetic method of D-p-methyl dibenzoyl tartaric acid, it comprises the steps:

[0050] Put 1.5kg of D-tartaric acid and 2L of toluene into a 10L three-necked bottle, add 20g of copper sulfate under stirring, start to add 3.5kg of p-toluoyl chloride dropwise, finish dropping in 3 hours, continue to react for 6 hours, and discharge to the centrifuge. Get 4.88kg of D-p-methyldibenzoyl tartaric anhydride by rejection filtration, put it into a 20L three-necked bottle, add 4.88kg of water and toluene each, heat up to reflux, keep for 5 hours, cool to normal temperature and discharge, and shake to obtain D- 3.71kg of p-methyldibenzoyl tartaric acid.

[0051] The D-p-methyldibenzoyl tartaric acid that present embodiment obtains is carried out TEM test, test structure such as figure 2 As shown, as can be seen from the figure, the purity content of finished product D-p-methyldibenzoyl tartaric acid is 99.76%, and the total yield is 95.9%.

[0052] Peak number Peak ...

Embodiment 3

[0073] A kind of synthetic method of D-p-methyl dibenzoyl tartaric acid, it comprises the steps:

[0074] Put 7.5kg of D-tartaric acid and 10L of toluene into a 50L reaction kettle, add 120g of copper sulfate under stirring, start to add 18kg of p-toluyl chloride dropwise, finish dropping in 4 hours, continue to react for 6 hours, discharge the material into a centrifuge, and shake Filter to get 24.9kg of D-p-methyldibenzoyl tartaric anhydride, put it into a 100L reactor, add 24.9kg of water and toluene, heat up to reflux, keep for 5 hours, cool to normal temperature and discharge, shake off to get D-p Methyl dibenzoyl tartaric acid 18.5kg.

[0075] The D-p-methyldibenzoyl 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-p-methyldibenzoyl tartaric acid purity content is 99.34%, and the total yield is 95.2%.

[0076] Peak Number Peak Name Retention Time Peak Pea...

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PUM

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Abstract

The invention discloses a Di-p-toluoyl-D-tartaric acid synthetic method. D-Tartaric acid and p-toluoyl chloride are taken as raw materials, copper sulfate is taken as a catalyst, toluene is taken as a solution, Di-p-toluoyl-D-tartaric anhydride is obtained through a reaction, an equivalent amount of water is added, and the toluene is hydrolyzed to obtain Di-p-toluoyl-D-tartaric acid, wherein the toluene solution, and water and the toluene in the hydrolysis can be recycled. The method is simple in process, safe and easy to operate, the process yield reaches over 95 percent; and at the same time, the cost of the raw materials is low, a part of raw material can be recycled, the purity of a finished product is high, and an excellent chiral resolution performance is achieved.

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-p-methyldibenzoyl tartaric acid. Background technique [0002] D-p-methyldibenzoyl tartaric acid is a white crystalline powder that easily absorbs water in the air and is soluble in organic solvents such as ethanol and methanol. Widely used in 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 35%, the product purity is lower, and the production cost is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/76C07C67/29
CPCC07C67/14C07C69/76
Inventor 李志军楚静波崔清海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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