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Refining process of laurinol and process for preparing lauromacrogol by using refined product as raw material

A technology of lauryl alcohol and refined products, which is applied in the field of medicine and chemical industry, can solve problems such as poor stability, and achieve the effects of improving stability, reducing moisture, and reducing impurities

Active Publication Date: 2021-10-22
BEIJING ENCHENG KANGTAI BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The object of the present invention is to provide a production process of lauromacrogol with simple operation, mild reaction conditions, and suitable for industrial scale production, so as to solve the problem of poor stability of the current lauromacrogol bulk drug and reduce storage difficulty and storage cost , improve the stability and quality of lauromacrogol API

Method used

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  • Refining process of laurinol and process for preparing lauromacrogol by using refined product as raw material
  • Refining process of laurinol and process for preparing lauromacrogol by using refined product as raw material
  • Refining process of laurinol and process for preparing lauromacrogol by using refined product as raw material

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Experimental program
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Effect test

Embodiment 1

[0051] The preparation of embodiment 1 lauryl alcohol refined product 1

[0052] 1) Add 1 kg of lauryl alcohol raw material, 1 kg of tetrahydrofuran and 1 kg of acetonitrile into the reaction vessel, raise the temperature to about 28° C., and stir until completely dissolved to obtain a reaction solution. 2) Cool the reaction solution to 0° C., stir and crystallize for 30 minutes, filter with suction, collect the filter cake, and obtain the intermediate white solid. 3) Put the intermediate white solid into a reaction vessel, slowly raise the temperature to 40°C, stir until it melts, distill under reduced pressure after complete melting, evaporate the residual organic solvent in the system, collect the distillation product, gradually raise the temperature to 90°C, and control The vacuum degree was -0.1MPa, and the vacuum distillation was carried out for 4 hours to obtain the remaining product, which was the refined product of lauryl alcohol 1.

[0053] The lauryl alcohol refine...

Embodiment 2

[0056] The preparation of embodiment 2 lauryl alcohol refined product 2

[0057] 1) Add 5 kg of lauryl alcohol (raw material), 5 kg of tetrahydrofuran and 5 kg of acetonitrile into a reaction vessel, raise the temperature to about 25° C., stir to completely dissolve, and obtain a reaction solution. 2) Cool the reaction solution to -2°C, stir and crystallize for 20 minutes, filter with suction, collect the filter cake, and obtain the intermediate white solid. 3) Put the intermediate white solid into the reaction vessel, slowly raise the temperature to 20°C, stir until it melts, distill under reduced pressure after complete melting, distill off the residual organic solvent in the system, collect the distillation product, and gradually raise the temperature to 80°C, Control the vacuum degree to ≤-0.1MPa, and distill under reduced pressure for 5 hours to obtain the remaining product, which is the refined product of lauryl alcohol 2.

[0058] The refined lauryl alcohol product 2 p...

Embodiment 3

[0061] The preparation of embodiment 3 lauryl alcohol refined product 3

[0062] 1) Add 10kg lauryl alcohol (raw material), 10kg tetrahydrofuran and 20kg toluene to the reaction vessel, raise the temperature to 30°C, stir to dissolve completely, and obtain the reaction solution; 2) Cool the reaction solution to -1°C, stir and crystallize for 30min, and filter with suction , the filter cake was collected to obtain the intermediate white solid. 3) Put the white solid of the intermediate into the reaction vessel, slowly raise the temperature to 40°C, stir and melt, and distill under reduced pressure after complete melting, collect the distillation product, gradually raise the temperature to 70°C, control the vacuum degree ≤ -0.1MPa, and distill under reduced pressure for 6h , to obtain the remaining product, which is the refined product of lauryl alcohol 3. The refined lauryl alcohol product 3 prepared in Example 3 was tested according to the requirements for related substances ...

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Abstract

The invention relates to a refining process of laurinol and a process for preparing lauromacrogol by using a prepared laurinol refined product as a raw material. According to the preparation process of the lauromacrogol, impurities in the lauromacrogol are effectively reduced, a dehydration step in a lauromacrogol synthesis process is reduced, and energy consumption is reduced, so that the preparation process is suitable for industrial production; all indexes of the prepared lauromacrogol meet the requirements of EP and Chinese pharmacopoeia, the lauromacrogol has good oxidation resistance and high temperature resistance, can be stably stored at room temperature in the presence of air, and solves the problem that an existing lauromacrogol product needs to be stored at low temperature under the protection of inert gas, and the stability of the lauromacrogol is improved; and the lauromacrogol can be stored without special packaging, so that the production, storage and transportation costs are greatly reduced, effective support is provided for the production of the lauromacrogol preparation, the medication expenditure of patients is greatly reduced, and the lauromacrogol is beneficial to the majority of patients.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a process for refining lauryl alcohol and a process for preparing lauryl alcohol from the refined product. Background technique [0002] Lauromacrogol (Lauromacrogol), also known as ethoxylate hardening alcohol, polydocanol, molecular formula C 12 h 25 (OCH 2 CH 2 ) n OH (n=9), is a polymer product obtained by polymerization of lauryl alcohol (fatty alcohol) and multiple ethylene oxides. It is currently the most widely used sclerosing drug in clinical practice in Europe and the United States. It is mainly used in varicose veins, venous malformations, Sclerotherapy of hemangiomas, internal hemorrhoids, cystic diseases, etc. [0003] The safety of lauromacrogol has been recognized by the international medical community. It is the only drug approved for sclerotherapy in Germany so far, and it has been used in other European countries. The U.S. Food and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/125C07C29/78C07C43/11C07C41/03A61K31/08A61P9/14A61P35/00
CPCC07C31/125C07C29/78C07C43/11C07C41/03A61P9/14A61P35/00Y02P20/52
Inventor 张晟源冯淑香李燕飞郭云珍王斌
Owner BEIJING ENCHENG KANGTAI BIOLOGICAL TECH
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