Preparation method of polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer

A technology of polyethylene glycol monomethyl ether and block copolymer, which is applied in the field of preparation of polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer, can solve problems such as reaction temperature limitation, and achieves simple operation. Convenience, production conditions are not harsh, and the effect of dispersion is soft

Active Publication Date: 2013-04-24
上海谊众药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the published literature, the use of solvent polycondensation method to prepare polyethylene glycol monomethyl ether-dl-polylactic acid block copolymers almost uniformly uses toluene, and the boiling point of toluene is only 115 ° C, so its reaction temperature during the reaction subject to certain restrictions

Method used

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  • Preparation method of polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer
  • Preparation method of polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0018] 1. Add one of cumene, xylene, anisole, dimethylformamide and dimethyl sulfoxide to a dry reactor according to Table 1. For example, add anisole three to five times the total amount of raw materials input in advance, then add the catalyst stannous octoate, and polyethylene glycol monomethyl ether 2000 and dl-lactide in a certain proportion according to Table 1. Stir to dissolve evenly. Nitrogen gas was passed through, and the air was removed. Then heat to react. The heating temperature is limited between 110°C and 180°C depending on the solvent used. The reaction time is then set between 4 hours and 12 hours. Then the reaction stops.

[0019] 2. Slowly pour the viscous reactants into the pasty mixture of petroleum ether-carbon dioxide dry ice while vigorously stirring. Place and filter to obtain a white solid. Dry in a vacuum oven at 40°C for 24 hours. A white solid of polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer was obtained.

[0020] ...

Embodiment 2

[0037] 1. Add one of cumene, xylene, anisole, dimethylformamide and dimethyl sulfoxide to the dry reactor respectively according to Table 1, such as the amount according to the preset ratio 3 to 5 times the cumene, add polyethylene glycol monomethyl ether 2000 and dl-lactide in a certain proportion according to Table 1 in sequence. Stir to dissolve evenly. After raising the temperature to 120°C, a catalytic amount of stannous octoate was added, and nitrogen gas was introduced to remove the air. Then heat to react. The heating temperature is limited between 120°C and 180°C depending on the solvent used. The reaction time is then set between 4 hours and 12 hours. Then the reaction stops.

[0038] 2. Distill under reduced pressure to remove the solvent under reduced pressure as much as possible. Add 2 to 8 times the amount of polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer as a good solvent such as dichloromethane or methanol, and stir to help it diss...

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Abstract

The invention belongs to the filed of biopolymer material synthesis, relates to a preparation method of a polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer. The method includes the following steps of: adding a solvent with volume more than 3-6 times of total weight of reagents into a dried reactor, adding stannous octoate as a catalyst, and polyethylene glycol monomethyl ether and dl-lactide whose weight ratio is in the range of 65:35 to 20:80, introducing nitrogen, removing air, then heating and reacting, pouring a product into a compound of petroleum ether-carbon dioxide dry ice, simultaneously, violently stirring, obtaining the needed product after drying a white filtered solid in a vacuum drying oven. The new-type solvent is used in the invention, and a novel purification processing method is provided and is simple and easily controlled, the copolymer with a certain amount of molecular weight can be synthesized according to the specified requirement, and the requirement of further producing a pharmaceutical preparation is met.

Description

technical field [0001] The invention belongs to the field of biopolymer material synthesis, and in particular relates to a preparation method of polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer. Background technique [0002] Polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer is a biodegradable material. Widely used in various pharmaceutical dosage forms. It has been reported in the literature that polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer eventually degrades into carbon dioxide and water in the human body. A certain molecular weight polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer can form micelles. After these micelles are prepared into pharmaceutical dosage forms with some raw materials, they have the advantages of sustained release, targeting, safety, easy absorption and less side effects. The methods for preparing and producing polyethylene glycol monomethyl ether-dl-polyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/664C08G63/81C08G63/90C08G65/48
Inventor 李端何毓嘉蒋新国刘斌卢瓛沈亚领
Owner 上海谊众药业股份有限公司
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