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PH sensitive solution polyacrylic acyloxy oxo acetate and its synthesis method

A technology of polyacryloyl hydroxamate and synthesis method, applied in the field of novel carrier polylacenoyl hydroxamate and its synthesis, can solve the problem that the pH sensitivity of hydroxamate is rarely studied and the like, and achieve a good pH Sensitive erodibility, the effect of a simple synthesis process

Inactive Publication Date: 2008-02-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few studies on the pH sensitivity of hydroxamate at home and abroad, and there is no report on the preparation of hydroxamate as a drug carrier material with acrylamide polymer as the main chain.

Method used

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  • PH sensitive solution polyacrylic acyloxy oxo acetate and its synthesis method
  • PH sensitive solution polyacrylic acyloxy oxo acetate and its synthesis method
  • PH sensitive solution polyacrylic acyloxy oxo acetate and its synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] First take monomer AM 0.14mol and initiator AIBN 1.2×10 -3 mol, placed in a 250ml three-necked flask, completely dissolved with 45ml of absolute ethanol and 45ml of acetone, stirred and blown with nitrogen for 30min, then heated to 60°C. When white turbidity appeared, the reaction was continued for 2.5 h, and the reaction was stopped. Cool, filter with suction, wash 3 times with absolute ethanol, and vacuum-dry at 40°C until constant weight. Take 0.12mol NH 2 OH·HCl and 0.2mol NaOH were dissolved in 150ml of distilled water to obtain a free hydroxylamine solution, and 0.1mol PAM was slowly added to dissolve it completely, then reacted in a constant temperature water bath at 90°C for 6 hours to obtain an aqueous solution of hydroxamic acid. Then add 0.12mol NaOH to the reaction system for preparing hydroxamic acid, add an equivalent amount of freshly distilled benzoyl chloride dropwise to the solution under vigorous stirring, and after the product is fully separated, f...

Embodiment 2

[0024] First take monomer AM 0.14mol and initiator AIBN 1.2×10 -3 mol, placed in a 250ml three-necked flask, completely dissolved with 45ml of absolute ethanol and 45ml of acetone, stirred and blown with nitrogen for 30min, then heated to 60°C. When white turbidity appeared, the reaction was continued for 2.5 h, and the reaction was stopped. Cool, filter with suction, wash 3 times with absolute ethanol, and vacuum-dry at 40°C until constant weight. Take 0.08mol NH 2 Dissolve OH·HCl and 0.15mol NaOH in 150ml distilled water to obtain free hydroxylamine solution, slowly add 0.1mol PAM, after complete dissolution, react in a constant temperature water bath at 90°C for 6 hours to obtain an aqueous solution of hydroxamic acid. Then add 0.08mol NaOH to the reaction system for preparing hydroxamic acid, add an equivalent amount of freshly distilled benzoyl chloride dropwise to the solution under vigorous stirring, and after the product is fully separated, centrifuge, wash with dist...

Embodiment 3

[0026] First, take monomer AM 0.14mol and initiator AIBN 1.2×10 -3 mol, placed in a 250ml three-necked flask, completely dissolved with 45ml of absolute ethanol and 45ml of acetone, stirred and blown with nitrogen for 30min, then heated to 60°C. When white turbidity appeared, the reaction was continued for 2.5 h, and the reaction was stopped. Cool, filter with suction, wash 3 times with absolute ethanol, and vacuum-dry at 40°C until constant weight. Take 0.05mol NH 2 OH·HCl and 0.12mol NaOH were dissolved in 150ml of distilled water to obtain a free hydroxylamine solution, and 0.1mol PAM was slowly added to dissolve it completely, then reacted in a constant temperature water bath at 90°C for 6 hours to obtain an aqueous solution of hydroxamic acid. Then add 0.05mol NaOH to the reaction system for preparing hydroxamic acid, add an equivalent amount of freshly distilled benzoyl chloride dropwise to the solution under vigorous stirring, and after the product is fully separated,...

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Abstract

The disclosed synthesis method for a polyacryloyl hydroxamate with structural formula as following (wherein, n=0-1700, m=3400-200, s=0-1450, q=3400-200; m:n=0-1, s:q=0-1)and strong pH sensitive corrosion as new enteric-soluble carrier material for oral administration comprises: dissolving the acrylamide, N-VP and initiator of azobisisobutyronitrile as given ratio in organic solvent; leading N2, heating; cooling to filter and clean in anhydrous ethanol; obtaining the polyacrylamide or N-VP / acrylamide copolymer by vacuum dry; dissolving some PAM or P (VP-co-AM) into the free hydroxylamine liquor to obtain the hydroxamic aqueous solution by thermostatic water-bath reaction; adding NaOH to stir and drip new-steamed acyl chloride; filtering, cleaning in distilled water till neutrality, and vacuum drying to obtain the final product.

Description

technical field [0001] The invention belongs to a compound synthesis method, and mainly relates to a novel carrier polyendenoyl hydroxamate with pH-sensitive erosion property and a synthesis method thereof. Background technique [0002] pH-sensitive materials are currently widely used drug carriers in oral enteric formulations. Generally, its types can be divided into two categories: one is enteric-coated materials represented by polyacrylic acid resin and cellulose acetate phthalate, which achieve the purpose of enteric coating through the increase of its water solubility in the intestinal pH environment [1 , 2]; another type of material refers to water-soluble polyelectrolytes, such as sodium alginate, polyacrylic acid, etc., which often contain drugs in the form of multivalent ion cross-linked hydrogels or polyelectrolyte complexes. The drug reaches the intestine for release and absorption in response to pH changes in the gastrointestinal tract or by gel-solution transit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/56C08F8/32C08F8/10C08F226/10A61K47/32
Inventor 邱利焱沈奇英
Owner ZHEJIANG UNIV
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