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Method for preparing dimethyl-beta-propiothetin

A technology of thiotin propionate and dimethyl, which is applied in the field of preparation and purification of dimethyl-β-thiotin propionate, an aquatic fish food attractant, can solve the problem of low content, unsuitable for large-scale production and use, and collection. The efficiency is not high, to achieve the effect of high product purity

Inactive Publication Date: 2017-11-24
宜兴市天石饲料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation methods of DMPT include natural extraction method and chemical synthesis method. The natural extraction method is to use algae plants as raw materials, and water is used as the extraction agent to extract dimethyl-beta-thiatin propionate in the algae plant body. Due to the low content of the extraction , and contains impurities, this method is not suitable for large-scale production and use; and the chemical synthesis method of halopropionic acid and methyl disulfide, the yield is not high

Method used

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  • Method for preparing dimethyl-beta-propiothetin

Examples

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Effect test

Embodiment 1

[0019] Example 1 Preparation of dimethyl-beta-thiatin propionate

[0020] a) Preparation of β-dimethylsulfonium propionic acid chloride (1)

[0021] Add 4mol 3-chloropropionic acid and 6mol dimethyl sulfide in the reaction flask, stir and heat to 40-50°C, so that 3-chloropropionic acid is dissolved in dimethyl sulfide, add 700ml of organic solvent acetone (in the specific During the operation, butanone or ethyl acetate can also be used instead of acetone as an organic solvent), keep stirring at 50°C for 20 hours, cool with a water bath to 25°C, and filter with suction. The filter cake was recrystallized with 1000ml of 95% (mass fraction) ethanol to obtain white crystal A, namely β-dimethylsulfonylpropionic acid chloride, weighing 156.5g.

[0022] b) Preparation of dimethyl-β-thiatin propionate (2)

[0023] Dissolve the white crystal A obtained in step a) in the smallest amount of water, then stir continuously, and slowly add 1 mol of sodium bicarbonate (in the specific imple...

Embodiment 2

[0025] a) Preparation of β-dimethylsulfonium propionic acid chloride (1)

[0026] Add 4mol 3-chloropropionic acid and 5.4mol dimethyl sulfide into the reaction flask, stir and heat to 40-50°C, so that 3-chloropropionic acid is dissolved in dimethyl sulfide, add 700ml of organic solvent butanone, Keep stirring at 50°C for 20 hours, cool in a water bath to 25°C, and filter with suction; the filter cake is recrystallized with 1000ml of 95% (mass fraction) ethanol to obtain white crystal A, weighing 145.3g.

[0027] b) Preparation of dimethyl-β-thiatin propionate (2)

[0028] Dissolve the above white crystal A in the minimum amount of water, then keep stirring, and slowly add 0.5 mol of sodium carbonate until no more gas is released, and after driving away the carbon dioxide, cool down to 0°C. Remove the sodium chloride generated by filtration, wash the filter cake with 100mL of dehydrated ethanol solvent, combine the solvent and the filtrate, then add 1.5L of anhydrous methanol ...

Embodiment 3

[0030] a) Preparation of β-dimethylsulfonium propionic acid chloride (1)

[0031] Add 4mol 3-chloropropionic acid and 5mol dimethyl sulfide into the reaction flask, stir and heat to 40-50°C to dissolve 3-chloropropionic acid in dimethyl sulfide, add 700ml of organic solvent ethyl acetate, Keep stirring at 50°C for 20 hours, cool in a water bath to 25°C, and filter with suction. The filter cake was recrystallized with 1000ml of 95% ethanol to obtain white crystal A with a weight of 135.3g.

[0032] b) Preparation of dimethyl-β-thiatin propionate (2)

[0033] Dissolve the above-mentioned white crystal A in the minimum amount of water, then keep stirring, and slowly add 1 mol of sodium hydroxide, measure the pH value of the solution at the same time, until the pH value no longer changes to the end of the reaction, cool down to 0 °C. Remove the generated sodium chloride by filtration, wash the filter cake with 100 mL of absolute ethanol solvent, combine the solvent and filtrate,...

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Abstract

The invention relates to a method for preparing dimethyl-beta-propiothetin (DMPT), and relates to the technical field of organic chemistry. The invention adopts a two-step synthesis method comprising the following steps: firstly, preparing beta-dimethyl mercaptopropionic acid chloride from chloropropionic acid and dimethyl sulfide; and then adding sodium bicarbonate for reaction, and recrystallizing and drying to obtain the DMPT. The invention adopts a unique synthesis method, wherein a yield of an intermediate product synthesized in a first step is 65-84%, and the purity of the product DMPT after purification can reach 96%; and the method provided by the invention is high in purity of the product, simple in synthesis step and suitable for popularization and application.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to the preparation and purification method of dimethyl-beta-thiatin propionate, an aquatic fish attractant. Background technique [0002] Dimethyl-β-thiatin propionate (DMPT) is a naturally occurring sulfur-containing compound, not only widely present in seaweed, but also in wild fish and shrimp, following amino acids, betaine, and glutamine The developed fourth-generation aquatic attractant has an attractant effect 1.25 times that of choline chloride, 2.56 times that of betaine, 1.42 times that of methylmethionine, and 1.56 times that of glutamine. Existing studies have shown that the growth-promoting effect of dimethyl-β-thiatin propionate (DMPT) is 2.5 times that of semi-natural bait without adding attractant, and it is used as a food attractant for aquatic animals. growth promoter , for various sea freshwater fish , The feeding behavior and growth of shrimp and crab...

Claims

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Application Information

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IPC IPC(8): C07C381/12
CPCC07C381/12
Inventor 邹益东邹苏燕邹三元朱建泉陈刚
Owner 宜兴市天石饲料有限公司
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