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Novel method for synthesizing allicin

A new method, the technology of allicin, is applied in the field of synthesis of diallyl trisulfide, the main component of allicin, and can solve the problem of low yield

Inactive Publication Date: 2020-05-05
JIANGSU QINGJIANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Allicin belongs to the medicine for the treatment of deep fungal and bacterial infections, such as fungal infections of the lungs and digestive tract, Candida albicans bacteremia, acute and chronic bacillary dysentery, acute and chronic enteritis, whooping cough, etc. It can also be used as a feed additive, food Odor enhancer, the synthetic method commonly used at present is to mainly adopt allyl chloride-sodium thiosulfate-sodium sulfide method to synthesize in the industry at present, but because reactant allyl chloride is insoluble in water, so the productive rate of two-phase reaction is relatively high. Low, the reaction equation is as follows:

Method used

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  • Novel method for synthesizing allicin
  • Novel method for synthesizing allicin
  • Novel method for synthesizing allicin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] The establishment of embodiment 1 synthetic route:

[0008] Add 36 g of sodium thiosulfate (containing 5 crystalline water) and 95 mL of distilled water into a 250 mL three-necked round-bottomed reaction flask with a magnetic stirring and reflux device, stir and heat up to about 35°C, then pipette 9.0 mL Allyl chloride was slowly dropped into the reaction flask in the dropping funnel, and the reaction temperature was controlled at 50±2°C to reflux. After reacting for 2 hours, cool to room temperature, and drop 10 mL of 1.8 mol / L sodium sulfide solution, stirred at room temperature for 30 min, the reaction solution was transferred to a separatory funnel, and stood overnight, discarded the lower water phase, washed the oil phase with distilled water for 3 times, and separated the water phase to obtain a light yellow oil, which was washed with anhydrous Na 2 SO 4 dry, filter out Na 2 SO 4 . Carry out vacuum distillation, collect fractions (59~60°C / 133.33 Pa), the cal...

Embodiment 2

[0010] The selection of embodiment 2 catalyst:

[0011] Add 36 g of sodium thiosulfate (containing 5 crystal water) and 95 mL of distilled water into a 250 mL three-necked round-bottomed reaction flask with a magnetic stirring and reflux device, stir and heat up to about 35 °C, add 0.05 g Phase-transfer catalyst tetra-n-butylammonium iodide, then pipette 9.0 mL of allyl chloride into the dropping funnel, slowly drop it into the reaction bottle, control the reaction temperature at 50±2°C and reflux, react for 2 h, cool After reaching room temperature, add 10 mL of 1.8 mol / L sodium sulfide solution dropwise into the reaction solution, stir at room temperature for 30 min, transfer the reaction solution into a separatory funnel, let it stand overnight, discard the lower aqueous phase, and wash the oil phase with distilled water 3 times, the water phase was separated to obtain a light yellow oil, which was washed with anhydrous Na 2 SO 4 dry, filter out Na 2 SO 4 , carry out va...

Embodiment 3

[0013] The selection of embodiment 3 catalyst concentration:

[0014] Add 36 g of sodium thiosulfate (containing 5 crystal water) and 95 mL of distilled water into a 250 mL three-necked round-bottomed reaction flask with a magnetic stirring and reflux device, stir and heat up to about 35 °C, add 0.1 g Phase-transfer catalyst tetra-n-butylammonium iodide, then pipette 9.0 mL of allyl chloride into the dropping funnel, slowly drop it into the reaction bottle, control the reaction temperature at 50±2°C and reflux, react for 2 h, cool After reaching room temperature, add 10 mL of 1.8 mol / L sodium sulfide solution dropwise into the reaction solution, stir at room temperature for 30 min, transfer the reaction solution into a separatory funnel, let it stand overnight, discard the lower aqueous phase, and wash the oil phase with distilled water 3 times, the water phase was separated to obtain a light yellow oil, which was washed with anhydrous Na 2 SO 4 dry, filter out Na 2 SO 4 ,...

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Abstract

The invention discloses a novel method for synthesizing allicin, which is technically characterized in that tetrabutylammonium bromide is used as a phase transfer catalyst for synthesizing diallyl trisulfide, so that the reaction time is shortened, and the yield is improved. The method has the advantages that, a problem in the prior art that the allyl chloride-sodium thiosulfate-sodium sulfide method is mainly adopted for synthesis in the industry at present, but the yield of the two-phase reaction is low due to the fact that the reactant allyl chloride is insoluble in water is solved. According to the method, tetrabutylammonium bromide, TBAI for short, is used as the phase transfer catalyst to synthesize diallyl trisulfide, so that the reaction time is shortened, the yield is increased, and the reaction equation is shown in the specification.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing diallyl trisulfide, the main component of allicin. Background technique [0002] Allicin belongs to the medicine for the treatment of deep fungal and bacterial infections, such as fungal infections of the lungs and digestive tract, Candida albicans bacteremia, acute and chronic bacillary dysentery, acute and chronic enteritis, whooping cough, etc. It can also be used as a feed additive, food Odor enhancer, the synthetic method commonly used at present is to mainly adopt allyl chloride-sodium thiosulfate-sodium sulfide method to synthesize in the industry at present, but because reactant allyl chloride is insoluble in water, so the productive rate of two-phase reaction is relatively low. Low, the reaction equation is as follows: [0003] [0004] The present invention uses tetrabutylammonium bromide, referred to as TBAI, as a phase transfer catalyst ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/24C07C321/18
CPCC07C319/24C07C321/18
Inventor 孙占奎邓玮章雪晴王崇益陈光
Owner JIANGSU QINGJIANG PHARMA
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