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Lauromacrogol refinement method

A refining method, the technology of lauromacrogol, which is applied in the field of medicine and chemical industry, can solve the problems affecting the safety and effectiveness of lauromacrogol, and achieve the effects of simple operation, improved product quality and high refining yield

Active Publication Date: 2014-07-16
NANJING CHIA TAI TIANQING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The presence of these impurities has seriously affected the safety and effectiveness of lauromacrogol
At present, there are few reports on the refining process of lauromacrogol. Only the patent of Shaanxi Tianyu Pharmaceutical Company (CN1762948A) discloses a preparation method of lauromacrogol. It uses sodium hydroxide as a catalyst, and after the crude product is polymerized, acetic acid is added. Adjust the pH to 5-7 to obtain a white or off-white ointment-like finished product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] a. Add 2.8kg of crude lauryl alcohol (the content of lauryl alcohol is 2.8%) into the reaction kettle, raise the temperature to 50°C, start stirring, program the temperature to 130°C, the heating rate is 2°C / min, and decompress at the same time Distillation operation. After the temperature reaches 130°C, continue vacuum distillation for 3 hours, and control the pressure at -0.08Mpa;

[0026] b. Naturally cool the above crude product to 90°C in the reaction kettle, and filter through a filter screen to obtain a light yellow viscous clear filtrate;

[0027] c. Cool the filtrate to 60°C naturally, and adjust the pH value of the system to about 7.0 with phosphoric acid while stirring the filtrate.

[0028] d. Continue to stir, carry out temperature programming at a rate of 2°C / min, and carry out vacuum distillation operation at the same time, the pressure is controlled at -0.08Mpa, after the temperature reaches 80°C, continue vacuum distillation for 2 hours to obtain the f...

Embodiment 2

[0030] a. Add 2.8kg of crude lauryl alcohol (the content of lauryl alcohol is 2.8%) into the reaction kettle, raise the temperature to 50°C, start stirring, program the temperature to 150°C, the heating rate is 20°C / min, and decompress at the same time Distillation operation. After the temperature reaches 150°C, continue vacuum distillation for 0.5 hours, and control the pressure at -0.08Mpa;

[0031] b. Naturally cool the above-mentioned crude product to 100°C in a reaction kettle, and filter through a filter screen to obtain a light yellow viscous clear filtrate;

[0032] c. Cool the above filtrate to 80°C naturally, and adjust the pH value of the system to about 7.5 with acetic acid while stirring the filtrate.

[0033] d. Continue to stir, carry out temperature program at a rate of 20°C / min, and carry out vacuum distillation operation at the same time, control the pressure at -0.08Mpa, after the temperature reaches 150°C, continue vacuum distillation for 0.5 hours to obta...

Embodiment 3

[0035] a. Add 2.8kg of crude lauryl alcohol (the content of lauryl alcohol is 2.8%) into the reaction kettle, raise the temperature to 50°C, start stirring, program the temperature to 130°C, the heating rate is 10°C / min, and decompress at the same time Distillation operation. After the temperature reaches 130°C, continue vacuum distillation for 9 hours, and control the pressure at -0.09Mpa;

[0036] b. Naturally cool the above crude product to 80°C in the reaction kettle, and filter through a filter screen to obtain a light yellow viscous clear filtrate;

[0037] c. Cool the above filtrate to 40°C naturally, and adjust the pH value of the system to about 7.5 with propionic acid while stirring the filtrate.

[0038] d. Continue to stir, carry out temperature programming at a rate of 10°C / min, and carry out vacuum distillation operation at the same time, the pressure is controlled at -0.08Mpa, after the temperature reaches 100°C, continue vacuum distillation for 10 hours to obt...

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Abstract

The invention relates to the field of pharmaceutical chemicals and in particular relates to a lauromacrogol refinement method. The method comprises the steps of performing reduced pressure distillation on a lauromacrogol crude product at certain temperature under certain pressure, filtering, adjusting the pH value of filter liquor, and performing reduced pressure distillation to obtain a high-purity lauromacrogol refinement product. The refinement method is simple and convenient to operate, mild in reaction condition and suitable for industrialized production and use.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and relates to a method for refining lauromacrogol 400 suitable for large-scale industrial production. Background technique [0002] Lauromacrogol 400 (Lauromacrogol 400), molecular formula C 12 h 25 (OCH 2 CH 2 ) 9 OH, is a class of anti-varicose drugs, the chemical name is α-isotridecyl-ω-hydroxy-poly(oxy-1,2-ethylene), and its structural formula is as follows: [0003] [0004] The drug was produced and launched by Shaanxi Tianyu Pharmaceutical Company in 2008. Due to its outstanding clinical efficacy and low side effects, it is widely used in clinical practice. Its preparation process mainly involves the polymerization reaction of lauryl alcohol and ethylene oxide through alkali catalysis, and the reaction formula is as follows: [0005] [0006] The crude lauryl alcohol synthesized by this preparation process contains two major types of impurities: the first type is ...

Claims

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Application Information

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IPC IPC(8): C07C43/13C07C41/34C07C41/42
CPCC07C41/34C07C41/42C07C43/11
Inventor 吴舰郭璇柴雨柱朱谧徐丹杨治旻田舟山
Owner NANJING CHIA TAI TIANQING PHARMA
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