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Novel synthesis method of D-dibenzoyl tartaric acid

A technology of dibenzoyl tartaric acid and a new method is applied in the directions of organic chemistry methods, chemical instruments and methods, carboxylate preparation, etc., and can solve the problems of strong irritation of raw materials, low utilization rate of raw materials, limitations in production and processing, etc. Easy operation, improved yield and product quality, mild conditions

Inactive Publication Date: 2017-11-17
ZHEJIANG JIAHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw materials are highly irritating, corrosive and toxic, and the utilization rate of raw materials is low, the production pollution is large, the yield is low, and the product purity is low
Although there is also an improved technology, the improved technology still uses toluene as a solvent, and it must be completed with D-tartaric acid. The use of the above-mentioned raw materials makes its production and processing limited

Method used

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  • Novel synthesis method of D-dibenzoyl tartaric acid

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Effect test

Embodiment 1

[0020] In the embodiment of the present invention, a new synthetic method of D-dibenzoyl tartaric acid comprises the following steps:

[0021] 1) Weigh tartaric acid and silicone oil, put them into a reaction kettle and stir for 40min at a temperature of 52°C. The mass volume ratio of tartaric acid and silicone oil is 1kg:8L; then, under stirring conditions of 100r / min, add ferric chloride, The addition of ferric chloride is 1% of tartaric acid quality. Then raise the temperature to 63°C, then continuously add benzamide to the reaction kettle in 3 minutes, and then continue to stir at this temperature for 2.3 hours to obtain mixed material A; the mass ratio of tartaric acid to benzamide is 1 :2.

[0022] 2) Add water equal to the volume of silicone oil to the mixture material A, stir at a stirring speed of 600r / min and a temperature of 80°C for 15 minutes, and after standing for 30 minutes, use a low-temperature high-speed centrifuge for centrifugation at a speed of 14000r / mi...

Embodiment 2

[0025] In the embodiment of the present invention, a new synthetic method of D-dibenzoyl tartaric acid comprises the following steps:

[0026] 1) Weigh tartaric acid and silicone oil, put them into a reaction kettle and stir for 50 minutes at a temperature of 55°C. The mass volume ratio of tartaric acid and silicone oil is 3kg:10L; then, under stirring conditions of 120r / min, add ferric chloride, The addition of ferric chloride is 3% of tartaric acid quality. Then raise the temperature to 68°C, then continuously add benzamide into the reaction kettle in 4min, and then continue to stir at this temperature for 2.5h to prepare mixed material A; the mass ratio of tartaric acid to benzamide is 1 :4.

[0027] 2) Add water equal to the volume of silicone oil to the mixture material A, stir for 20 minutes at a stirring speed of 800r / min and a temperature of 82°C, and after standing for 30 minutes, use a low-temperature high-speed centrifuge for centrifugal separation at a centrifugal...

Embodiment 3

[0030] In the embodiment of the present invention, a new synthetic method of D-dibenzoyl tartaric acid comprises the following steps:

[0031] 1) Weigh tartaric acid and silicone oil, put them into a reaction kettle and stir for 45min at a temperature of 54°C. The mass volume ratio of tartaric acid and silicone oil is 2kg:9L; then, under stirring conditions of 110r / min, add ferric chloride, The addition of ferric chloride is 2% of tartaric acid quality. Then raise the temperature to 65°C, then continuously add benzamide to the reaction kettle in 4 minutes, and then continue to stir at this temperature for 2.4 hours to obtain mixed material A; the mass ratio of tartaric acid to benzamide is 1 :3.

[0032] 2) Add water equal to the volume of silicone oil to the mixture material A, stir at a stirring speed of 700r / min and a temperature of 81°C for 18min, and after standing for 30min, use a low-temperature high-speed centrifuge to centrifuge and separate at a centrifugal speed of...

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Abstract

The invention discloses a novel synthesis method of D-dibenzoyl tartaric acid. The synthesis method comprises the following steps: weighing tartaric acid and silicone oil, adding tartaric acid and silicone oil into a reactor, stirring tartaric and silicone oil for 40 to 50 minutes at a temperature of 52 to 55 DEG C, wherein the ratio of tartaric acid to silicone oil is 1-3 kg: 8-10 L; adding ferric trichloride under stirring, heating to a temperature of 63 to 68 DEG C, continuously adding benzoyl amide into the reactor within 3-4 minutes, stirring for 2.3 to 2.5 hours at a temperature of 63 to 68 DEG C to obtain a mixed material A; adding water with a same volume of silicone oil into the mixed material A, stirring for 15 to 20 minutes at a stirring speed of 600-800 r / min at a temperature of 80-82 DEG C, allowing the system to stand still for 30 minutes, and carrying out centrifugal separation, wherein the precipitates are D-dibenzoyl tartaric acid. The technology is simple, the operation is convenient, and the conditions are mild. The safety and operability of the technology are improved. The environmental pollution is reduced, the synthesis method is suitable for large scale production; the time is shortened, the product yield and product quality are improved, and the chiral splitting performance is excellent.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a new method for synthesizing D-dibenzoyltartaric acid. Background technique [0002] D-dibenzoyl tartaric acid, a white crystalline powder, is widely used in the chiral resolution of amine compounds, and is also used as an intermediate of the anthelmintic drug levamisole (for resolution). The existing production method is obtained by hydrolyzing D-tartaric acid, benzoyl chloride and thionyl chloride as raw materials, using toluene as a solvent, and the yield is only 40%. The raw materials are highly irritating, corrosive, and highly toxic, and the utilization rate of raw materials is low, the production pollution is large, the yield is low, and the product purity is low. Although there is also improved technology, improved technology still adopts toluene as solvent, and must use D-tartaric acid to complete, and the use of the above-mentioned raw materials makes its p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/20C07C69/78
CPCC07B2200/07C07C67/20C07C69/78
Inventor 周少华陈江苏林世清范莲生徐俊平范素珍许康林
Owner ZHEJIANG JIAHUA CHEM
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