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Method for preparing hydroxypropyl methylcellulose acetate succinate

A technology of hydroxypropyl methylcellulose and hypromellose acetate, which is applied in the field of preparation of hypromellose acetate succinate, can solve the problems of many by-products, slow acylation reaction rate, and poor water resistance, and achieve The effect of speeding up the reaction rate, speeding up the reaction speed, and shortening the reaction time

Inactive Publication Date: 2012-12-05
美信佳中维药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The presence of an appropriate amount of acetyl groups will improve the flexibility of the free film of the HPMCAS coating material, improve acid resistance, and prevent the material from agglomerating and cohesively. The ratio should be such that the resulting acetyl content is not too high
The presence of succinyl group will improve the solubility of the free film of HPMCAS coating material, but if the content of succinyl group obtained by adding succinic anhydride is too high, it will have poor water resistance, poor acid resistance, and the pH value of the solution will decrease.
[0004] US4385078 (1983-5-23) provides a kind of preparation method of HPMCAS, but the acylation reaction rate of this method is slow, the reaction time is long, and by-product is many

Method used

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  • Method for preparing hydroxypropyl methylcellulose acetate succinate
  • Method for preparing hydroxypropyl methylcellulose acetate succinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 100g of hydroxypropyl methylcellulose, 10g of anhydrous sodium acetate and 20g of glacial acetic acid, stir and mix evenly, then add 25g of succinic anhydride and 30g of acetic anhydride; microwave the mixture for 4min under 400kw power, and naturally Cool to 50°C to obtain the reaction product; pour the reaction product into water, and after the reaction product is completely precipitated, wash and suction filter until the precipitated liquid is neutral; dry the filter cake obtained by suction filtration in a vacuum oven at 80°C, Obtain hypromellose acetate succinate, and the yield is shown in Table 1.

[0031] The product was analyzed by infrared, the results are shown in figure 1 . The absorption range of carboxylic acid (-COOH-) and carboxylic acid (-COO-) groups is 1720-1770cm -1 , figure 1 shows that at a wavenumber of 1740 cm -1 Strong sharp absorption peaks can be found at 1069, 1139 cm -1 The absorption peak at is confirmed to be the C-O-C stretching...

Embodiment 2

[0035] Take 100g of hydroxypropyl methylcellulose, 50g of anhydrous sodium acetate and 60g of glacial acetic acid, and mix them ultrasonically for 10 minutes, then add 75g of succinic anhydride and 50g of acetic anhydride; microwave the mixture at 750kw for 7 minutes, and cool it naturally The reaction product was obtained at 70°C; the reaction product was poured into water, and after the reaction product was completely precipitated, it was washed and suction filtered until the precipitated liquid was neutral; the filter cake obtained by suction filtration was dried in a vacuum oven at 80°C to obtain Hypromellose Acetate Succinate.

[0036]

Embodiment 3

[0038] Take 100g of hydroxypropyl methylcellulose, 40g of anhydrous sodium acetate and 30g of glacial acetic acid, and mix them ultrasonically for 8 minutes, then add 30g of succinic anhydride and 38g of acetic anhydride, and then stir for 5-8 minutes; microwave the mixture at a power of 500kw After 6 minutes of radiation, naturally cool to 50-70°C to obtain the reaction product; pour the reaction product into water, and after the reaction product is completely precipitated, wash and suction filter until the precipitated liquid is neutral; filter the filter cake obtained by suction filtration at 80 °C in a vacuum oven to obtain hypromellose acetate succinate.

[0039]

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Abstract

The invention relates to a method for preparing hydroxypropyl methylcellulose acetate succinate, and belongs to the field of chemical synthesis. The method comprises the following steps of: (1) preparing 100 weight parts of hydroxypropyl methylcellulose, 10 to 50 weight parts of anhydrous sodium acetate and 20 to 60 weight parts of glacial acetic acid, mixing, and adding 25 to 75 weight parts of succinic anhydride and 30 to 50 weight parts of acetic anhydride; (2) performing microwave radiation on the mixture obtained in the step (1) for 4 to 7 minutes under the power of 400 to 750 kw, and cooling naturally to the temperature of between 50 and 70 DEG C to obtain a reaction product; (3) pouring the reaction product into water, and after precipitating the reaction product completely, washing and performing suction filtration until precipitated liquid is neutral; and (4) drying filter cakes obtained by the suction filtration under vacuum to obtain the hydroxypropyl methylcellulose acetate succinate. The method is high in speed of acylation reaction, short in reaction time and few in byproducts.

Description

technical field [0001] The invention relates to a preparation method of hypromellose acetate succinate, which belongs to the field of chemical synthesis. Background technique [0002] Hydroxypropylmethylcellulose acetate succinate (HPMCAS) is a mixed ester of acetic acid and succinic acid of hydroxypropylmethylcellulose (HPMC), which is obtained by esterifying HPMC with acetic anhydride and succinic anhydride. Excellent enteric coating material. In addition to being used for enteric coating, it can also be used as a polymer carrier to prepare drug microcapsules, microspheres and drug slow-release or controlled-release preparations. As an enteric coating material, it is characterized by good film-forming properties, no need to add plasticizers, and good solubility in the upper small intestine. [0003] HPMCAS contains methoxy, hydroxypropoxy, acetyl and succinyl groups. Wherein the methoxyl group is a hydrophobic group, if the methoxyl content is too small, HPMCAS will be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B13/00
Inventor 费玉元
Owner 美信佳中维药业股份有限公司
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