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Synthesis method of cystamine dihydrochloride

A technology of cystamine dihydrochloride and cystamine dihydrochloride, which is applied in the field of solid-phase synthesis of cystamine dihydrochloride at room temperature, can solve the problems of high production cost and complicated production process, and achieve the effect of low cost

Active Publication Date: 2012-04-04
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] The existing method for synthesizing cystamine dihydrochloride is to use an oxidizing agent to oxidize cysteamine hydrochloride. The reaction needs to be carried out in the liquid phase, requires precise temperature control, and requires a complete set of liquid phase reaction equipment. The production process is complicated and the production cost is low. higher

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  • Synthesis method of cystamine dihydrochloride
  • Synthesis method of cystamine dihydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 864g of composite glue, 1620g of water, 4320g of cysteamine hydrochloride, 2376g of 120 mesh powdered silicon dioxide and 1620g of aminobutyric acid, add the composite glue to water, add cysteamine hydrochloride, stir evenly, and place at room temperature 2h, grind twice with a colloid mill, add silica to absorb into solid powder, finally add aminobutyric acid and stir for 10min, place in the container at room temperature of 25°C for 62h, the internal temperature of the material is consistent with the ambient temperature, and the reaction is completed. The reaction product was dissolved in water and filtered, and the filtrate was purified with ethanol to obtain pure cystamine dihydrochloride. The composition of the composite glue is 258g of carboxymethyl cellulose, 172g of sodium alginate and 430g of xanthan gum.

[0019] The infrared spectrogram of cystamine dihydrochloride prepared after the purification of the reaction product of this embodiment is as follows ...

Embodiment 2

[0021] Weigh 860g of composite glue, 2150g of water, 1720g of cysteamine hydrochloride, 3010g of 80 mesh powdered silicon dioxide and 860g of aminobutyric acid, add the composite glue to water, add cysteamine hydrochloride, stir evenly, and place at room temperature 3h, grind twice with a colloid mill, add silica to absorb into solid powder, finally add aminobutyric acid and stir for 10min, place in a container at room temperature of 35°C for 48h, the internal temperature of the material is consistent with the ambient temperature, and the reaction is completed. The reaction product was dissolved in water and filtered, and the filtrate was purified with ethanol to obtain pure cystamine dihydrochloride. The composition of the composite gum is 345.6 g of carboxymethyl cellulose, 259.2 g of sodium alginate and 259.2 g of xanthan gum.

[0022] After the reaction product was purified, it was identified as cystamine dihydrochloride by infrared spectrum analysis, and the reduction and...

Embodiment 3

[0024] Weigh 59.5g of composite glue, 1190g of water, 2975g of cysteamine hydrochloride, 1666g of 150 mesh powdered silicon dioxide and 59.5g of aminobutyric acid, add the composite glue to water, add cysteamine hydrochloride, stir evenly, Place at room temperature for 3 hours, grind once with a colloid mill, add silica to absorb into solid powder, and finally add aminobutyric acid and stir for 10 minutes, place in a container at room temperature at 15°C for 120 hours, and the internal temperature of the material is consistent with the ambient temperature, and the reaction is completed. The reaction product was dissolved in water and filtered, and the filtrate was purified with ethanol to obtain pure cystamine dihydrochloride. The composition of the composite gum is 29.75 g of carboxymethyl cellulose, 5.95 g of sodium alginate and 23.8 g of xanthan gum.

[0025] After purification, the reaction product was identified as cystamine dihydrochloride by infrared spectrum analysis, ...

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Abstract

The invention provides a synthesis method of cystamine dihydrochloride. The method comprises the following steps of: 1, weighing the following components in percentage by mass: 20-50% of cysteamine hydrochloride, 15-25% of water, 1-10% of compounded latex, 22-35% of adsorbent and 1-15% of catalyst; 2, adding the compounded latex in the step 1 in water, adding cysteamine hydrochloride and uniformly stirring, standing for 2-3 hours at room temperature; milling once or twice by a colloid mill; adding the absorbent for absorbing so as to obtain solid powder; finally adding the catalyst and stirring uniformly, wherein the catalyst is aminobutyric acid; standing in a container for 48-120 hours at room temperature till the internal temperature of the materials is identical to the room temperature and the reaction is finished; dissolving reaction products with water and filtering, purifying the filtrate with ethanol and precipitating to obtain pure cystamine dihydrochloride. The synthesis method is a solid-phase room-temperature synthesis and has the advantages of simple process, less investment in equipment and low production cost.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a method for synthesizing cystamine dihydrochloride in solid phase at room temperature. Background technique [0002] Cystamine dihydrochloride is an important pharmaceutical intermediate, used in the synthesis of heparin antagonists, fructose bisphosphatase, coenzyme A, etc. Cystamine dihydrochloride is a commonly used drug in the treatment of radiation sickness. The latest research shows that it has a good blood circulation effect, can slowly and continuously promote the expansion of capillary smooth muscle, and increase the blood supply of microcirculation. [0003] The existing method for synthesizing cystamine dihydrochloride is to use an oxidizing agent to oxidize cysteamine hydrochloride. The reaction needs to be carried out in the liquid phase, requires precise temperature control, and requires a complete set of liquid phase reaction equipment. The production...

Claims

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Application Information

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IPC IPC(8): C07C323/25C07C319/24
Inventor 李永富史锋
Owner JIANGNAN UNIV
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