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A method for catalyzing and synthesizing glyceryl behenate for pharmaceutical excipients

A technology of glyceryl behenate and pharmaceutical excipients, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve problems such as long reaction time, low yield, and easily exceeded acid value. Achieve the effect of short reaction time, simple operation and convenient post-processing

Active Publication Date: 2020-11-06
WUHAN JASON BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the actual production process, this method has the following problems: the reaction time is too long, and the color needs to be decolorized if the color is dark, but in fact the decolorization is almost impossible to remove, the yield is also low, and the acid value is also easy to exceed the standard

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 34.1 kg of behenic acid, 5.58 kg of glycerin (mole ratio 1.65:1) and 0.4 kg of zinc oxide (1% of the total amount) into a 250-liter reactor in sequence, and heat to 120°C under nitrogen protection to melt into a clear and transparent liquid , turn on the vacuum pump, keep the pressure at -0.095MPa, and finish the reaction after 3 hours of heat preservation at 120°C. When the temperature is slowly lowered to 70°C, add 200 kg of ethyl acetate to dissolve, add hydrochloric acid to neutralize the solution until the solution is clear, and use 20 kg of purified water to wash the two The second time, the organic layer was cooled to 15°C to crystallize, centrifuged, the filter cake was washed with water to pH=7, dried in vacuum and pulverized to obtain 37.20 kg of white powder product with a yield of 98.7%, a melting point of 75°C, an acid value of 2.1, and an iodine value of 0.3. Saponification value 151, monoglyceride behenate 15.4%.

Embodiment 2

[0032] Add 34.1 kg of behenic acid, 5.58 kg of glycerol (1.65:1 molar ratio) and 0.6 kg of iron oxide (1.5% of the total amount) into a 250-liter reactor in sequence, and heat to 130°C under nitrogen protection to melt into a clear and transparent liquid , turn on the vacuum pump, maintain the pressure at -0.095MPa, keep the temperature at 130°C for reaction, and the reaction ends after 5 hours. When the temperature is slowly lowered to 60°C, add 200 kg of ethyl acetate to dissolve, add hydrochloric acid to neutralize the solution until the solution is clear, and wash with 30 kg of purified water. Twice, the organic layer was cooled to 15°C to crystallize, centrifuged, the filter cake was washed with water until pH = 7, vacuum dried and pulverized to obtain 36.7 kg of white powder product, yield 96.9%, melting point 75°C, acid value 2.8, iodine value 0.8 , saponification value 154, monoglyceride behenate 15.0%.

Embodiment 3

[0034]Put 34.1 kg of behenic acid, 5.58 kg of glycerin (molar ratio 1.65:1) and 0.4 kg of barium oxide (1% of the total amount) into a 250-liter reactor in sequence, and heat to 130°C under nitrogen protection to melt into a clear and transparent liquid , turn on the vacuum pump, maintain the pressure at -0.095MPa, and finish the reaction after 6 hours of heat preservation at 130°C. Slowly cool down to 70°C, add 220 kg of ethyl acetate to dissolve, add hydrochloric acid to neutralize the solution until the solution is clear, use 40 kg of purified water to wash the two The second time, the organic layer was cooled to 10°C to crystallize, centrifuged, the filter cake was washed with water to pH=7, dried in vacuum and pulverized to obtain 36.1 kg of white powder product with a yield of 95.8%, a melting point of 74°C, an acid value of 2.7, and an iodine value of 0.9. Saponification value 150, monoglyceride behenate 14.6%.

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Abstract

The invention discloses a catalysis and synthesis method of glyceryl behenate for a pharmaceutical aid, belonging to the technical field of synthesis of pharmaceutical aids. The method comprises the steps of adding behenic acid, glycerol and metal oxide into a reaction kettle, raising temperature to 80 DEG C-150 DEG C under vacuum stirring and performing dehydration esterification reaction, after reaction, adding ethyl acetate and other solvents to dissolve, neutralizing a catalyst with acid and then washing with water, cooling, crystalizing, filtering and drying an obtained organic layer so as to obtain the product, wherein the solid metal oxide is selected from one or more of zinc oxide, calcium oxide, aluminum oxide, magnesium oxide, iron oxide, copper oxide, barium oxide, and titanium dioxide. The method adopts metal oxide catalytic esterification reaction, is carried out at low temperature, is short in reaction time, and is convenient in post-treatment. The obtained product is pure white powder, all indexes of the product are within the pharmacopoeia range, and the yield of the product is 95% or more. The method is simple to operate, and is very suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of synthesis of pharmaceutical excipients, in particular to a method for catalytically synthesizing glyceryl behenate used as pharmaceutical excipients. The method uses metal oxides as catalysts, and the synthesized glyceryl behenate contains three kinds of esters at the same time. And the content of monoglyceride behenate is 12%-18%. The method has the advantages of low reaction temperature, short reaction time and light color of the product. Background technique [0002] Glyceryl behenate is a white powder obtained by esterification of behenic acid and glycerin. The main components are a mixture of monoglyceride behenate, diglyceride behenate and triglyceride behenate. The content of monoglyceride behenate in excipient grade glyceryl behenate is 12%-18%, and the acid value is below 4. It is a nonionic surfactant with good lubricating, emulsifying, and matrix slow-release properties. Because it is a mixtur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/30
CPCC07C67/08C07C69/30
Inventor 唐启明张进军李健雄汪川黄发勋
Owner WUHAN JASON BIOTECH CO LTD
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