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Method for synthesizing dithiothreitol

A technology of dithiothreitol and a synthesis method, applied in the field of compound synthesis, can solve the problems of difficult separation and purification of DTT, unsuitable for industrialized production, high production cost, etc., and achieves the avoidance of isomer impurities and the simplicity of separation and purification. effect of improving productivity

Inactive Publication Date: 2009-08-12
CHONGQING BORNING CHEM & INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The defect of this method is that: when generating the thio intermediate, an isomer impurity of DTT will be generated, the physical and chemical properties of this impurity are very similar to DTT, which will lead to the difficulty of separation and purification of DTT, low yield and low production cost. Expensive, only suitable for laboratory synthesis, not suitable for industrial production

Method used

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  • Method for synthesizing dithiothreitol
  • Method for synthesizing dithiothreitol
  • Method for synthesizing dithiothreitol

Examples

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Embodiment 1

[0026] The synthetic method of the DTT of the present embodiment, calculates raw material consumption according to product theoretical production amount 277.6g, comprises the following steps:

[0027] a. Add 162.5g (1.80mol) of 1,4-butenediol into the reaction kettle, slowly add 316.8g (1.98mol) of liquid bromine dropwise under stirring condition, and stir the reaction at a temperature of 25°C after the dropwise addition After 16 hours, let it stand for stratification, and take the supernatant to obtain 2,3-dibromo-1,4-butanediol, store it in a storage tank with a temperature lower than 30°C, and store it for later use;

[0028] b. Add 651.2 g (4.88 mol) of 30% sodium hydroxide solution to the supernatant obtained in step a, and stir and react for 16 hours at a temperature lower than 20° C. to obtain dioxirane alkyl;

[0029] c. In the reaction solution obtained in step b, add 155.67 g (2.045 mol) of thioacetic acid, stir and react for 20 hours, distill under reduced pressure...

Embodiment 2

[0032] The synthetic method of the DTT of the present embodiment, calculates raw material consumption according to product theoretical production amount 277.6g, comprises the following steps:

[0033] a. Add 162.5g (1.80mol) of 1,4-butenediol into the reaction kettle, slowly add 331.2g (2.07mol) of liquid bromine dropwise under stirring condition, and stir the reaction at a temperature of 27°C after the dropwise addition After 16 hours, let it stand for stratification, and take the supernatant to obtain 2,3-dibromo-1,4-butanediol, store it in a storage tank with a temperature lower than 30°C, and store it for later use;

[0034] b. In the supernatant obtained in step a, add 712.2 g (5.70 mol) of sodium hydroxide solution with a mass percentage concentration of 32%, and stir and react for 16 hours at a temperature lower than 20 ° C to obtain dioxirane alkyl;

[0035] c. In the reaction solution obtained in step b, add 159.38 g (2.094 mol) of thioacetic acid, stir and react for...

Embodiment 3

[0038] The synthetic method of the DTT of the present embodiment, calculates raw material consumption according to product theoretical production amount 277.6g, comprises the following steps:

[0039] a. Add 162.5g (1.80mol) of 1,4-butenediol into the reaction kettle, slowly add 345.6g (2.16mol) of liquid bromine dropwise under stirring conditions, and stir the reaction at a temperature of 30°C after the dropwise addition After 16 hours, let it stand for stratification, and take the supernatant to obtain 2,3-dibromo-1,4-butanediol, store it in a storage tank with a temperature lower than 30°C, and store it for later use;

[0040] b. In the supernatant obtained in step a, add 755.0 g (6.512 mol) of sodium hydroxide solution with a mass percent concentration of 34.5%, and stir and react for 16 hours at a temperature lower than 20°C to obtain dioxirane alkyl;

[0041] c. In the reaction solution obtained in step b, add 163.01 g (2.143 mol) of thioacetic acid, stir and react for ...

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Abstract

The invention discloses a synthesizing method of dithiothreitol. 1,4-butylene glycol is used as an initiating raw material and undergoes addition reaction with bromine at first to obtain 2,3-dibromo-1,4-butylene glycol; hydrolyzation under the catalyzation of alkali is carried out to obtain dioxirane; addition reaction with thioacetic acid is carried out to obtain dithiothreitol diacetate; and finally hydrolyzation under the catalyzation of alkali is carried out to obtain the dithiothreitol. The synthesizing method avoids the generation of dithiothreitol isomeride impurities, simplifies the product separation and purification, and can improve the yield rate, greatly reduce the production cost and is applicable to industrial production.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a synthesis method of dithiothreitol. Background technique [0002] Dithiothreitol (DL-Dithiothreitol, referred to as DTT) is a small molecule organic reducing agent, the chemical formula is C 4 h 10 o 2 S 2 , is mainly used in the field of biotechnology as a protein cleavage reagent. [0003] At present, the most widely used DTT synthesis method is to use threitol as a raw material, first oxidize with potassium permanganate, then obtain a thio intermediate under the action of thioacetic acid, and finally hydrolyze the thio intermediate to obtain DTT. The defect of this method is that: when generating the thio intermediate, an isomer impurity of DTT will be generated, the physical and chemical properties of this impurity are very similar to DTT, which will lead to the difficulty of separation and purification of DTT, low yield and low production cost. Expensive, only suitable f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/12C07C319/08
Inventor 余汶檑
Owner CHONGQING BORNING CHEM & INDAL
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