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Method for synthesizing high-purity batyl alcohol

A high-purity technology of batyl alcohol, which is applied in the field of medicine, can solve the problems of high residual amount of batyl alcohol solvent, large toxic and side effects, etc., and achieve the effect of simple and fast synthesis route and no toxic and side effects

Inactive Publication Date: 2018-12-14
JIANGSU PENGYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The main synthesis method of batalinol products currently on the market is to utilize 1,2-isopropylidene glyceryl ether and stearyl alcohol-p-toluenesulfonate to form ether in potassium hydroxide and toluene, and then hydrolyze acetone to obtain the finished product. The content is about 97%. The residue of batalyl alcohol solvent obtained by this method is relatively high, and the toxic and side effects are large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add methyl stearate, glycerin, methanol and ethanol into the container, the mass ratio of the four is 4:1.5:2:1, add hydrochloric acid solution dropwise under stirring at 0°C, the amount of hydrochloric acid solution added is 1 / 1 of the mass of ethanol 2. After the dropwise addition, raise the temperature to 50°C, keep the temperature for reaction for 2 hours, stop the reaction when the content of methyl stearate ≤ 0.1%, and obtain the crude batyl alcohol; slowly add ethanol to the crude batyl alcohol, the amount of ethanol added It was 5 times the amount of ethanol added in the preparation of the aforementioned crude product, and the temperature was raised to 40°C for 2 hours, and then n-hexane with the same mass as the glycerol in the preparation of the aforementioned crude product was added to cool, crystallize, suction filter, and dry to obtain the finished batyl alcohol.

Embodiment 2

[0015] Add methyl stearate, glycerin, methanol and ethanol into the container, the mass ratio of the four is 4:1.6:2:1, add hydrochloric acid solution dropwise under stirring at 0°C, the amount of hydrochloric acid solution added is 1 / 1 of the mass of ethanol 2. After the dropwise addition, raise the temperature to 55°C, keep the temperature for reaction for 3 hours, stop the reaction when the content of methyl stearate ≤ 0.1%, and obtain the crude batyl alcohol; slowly add ethanol to the crude batyl alcohol, the amount of ethanol added The amount of ethanol added in the preparation of the aforementioned crude product was 6 times that of ethanol, and the temperature was raised to 45°C for 3 hours, and then n-hexane with the same mass as the glycerin used in the preparation of the aforementioned crude product was added for cooling, crystallization, suction filtration, and drying to obtain the finished batyl alcohol.

Embodiment 3

[0017] Add methyl stearate, glycerin, methanol and ethanol into the container, the mass ratio of the four is 4:1.5:2:1, add hydrochloric acid solution dropwise under stirring at 0°C, the amount of hydrochloric acid solution added is 1 / 1 of the mass of ethanol 2. After the dropwise addition, raise the temperature to 52°C, keep the temperature for reaction for 2.5 hours, stop the reaction when the content of methyl stearate ≤ 0.1%, and obtain the crude batyl alcohol; slowly add ethanol to the crude batyl alcohol, and add ethanol The amount is 5.5 times the amount of ethanol added in the preparation of the aforementioned crude product, and the temperature is raised to 43°C to react for 2.5 hours, and then add n-hexane with the same quality as glycerol in the preparation of the aforementioned crude product for cooling, crystallization, suction filtration, and drying to obtain the finished batyl alcohol .

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Abstract

The invention discloses a method for synthesizing high-purity batyl alcohol. The method comprises the following steps: obtaining a crude batyl alcohol product from methyl stearate and glycerol as rawmaterials by catalyst hydrolysis, and then crystallizing crude batyl alcohol product by n-hexane and ethanol to obtain high-purity batyl alcohol. The finished batyl alcohol product produced with the method has impurity content less than 0.3% and has no toxic or side effects, and the synthesis route is simple and quick; according to the standard of the national Ministry of health, the content of shark batyl alcohol C21H44O3 is not less than 97.0% in terms of dry active pharmaceutical ingredients of batyl alcohol, while the content of batyl alcohol prepared with the method is higher than or equal to 99.8%, and the melting point is 72.6-73 DEG C, which is superior to the national standard.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a method for synthesizing high-purity batyl alcohol. Background technique [0002] Bakeloid alcohol is isolated from shark cod liver oil, and it also exists in animal yellow bone marrow. Bakelyl alcohol is an inherent substance in animals, and its content is relatively high in bone marrow hematopoietic tissues. It has the effect of promoting white blood cell proliferation and anti-radiation, and can also be used to improve leukopenia caused by solid benzene poisoning and radiopharmaceuticals. Its chemical name is: 3-(octadecyloxy)-1,2-propanediol, that is, ɑ-n-octadecylglycerol ether, and its chemical formula is——C 21 h 44 o 3 , can increase the number of megakaryocytes and granulocytes decreased by radiation, and can prolong the survival period. It has the effect of promoting white blood cell proliferation and anti-radiation, and can prevent and treat leukopenia. It can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/13
CPCC07C41/16C07C43/13
Inventor 陈梦琦侯珂兰张添程蒋锋周健
Owner JIANGSU PENGYAO PHARMA
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