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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, which can solve the problems of reaction temperature limitation and achieve simple operation Convenience, small loss and high yield

Active Publication Date: 2011-10-19
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

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Embodiment 1

[0018] 1. Add one of the solvents of cumene, xylene, anisole, dimethylformamide, and dimethyl sulfoxide into a dry reactor according to Table 1. For example, adding three to five times the total amount of anisole according to the preset raw material input, adding the catalyst stannous octoate, and a certain proportion of polyethylene glycol monomethyl ether 2000, dl-lactide according to Table 1. Stir and dissolve evenly. Add nitrogen to remove air. Then it is heated to react. The heating temperature is limited to 110°C and 180°C depending on the solvent used. The reaction time is then set between 4 hours and 12 hours. Then stop the reaction.

[0019] 2. Slowly pour the viscous reactant into the petroleum ether-carbon dioxide dry ice paste mixture while stirring vigorously. Place and filter to get 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] 3. The str...

Embodiment 2

[0036] 1. Add one of the solvents of cumene, xylene, anisole, dimethylformamide, and dimethyl sulfoxide into the dry reactor according to Table 1, such as the amount according to the preset ratio 3 to 5 times the cumene, followed by adding polyethylene glycol monomethyl ether 2000 and dl-lactide in a certain proportion according to Table 1. Stir and dissolve evenly. After the temperature was raised to 120°C, a catalytic amount of stannous octoate was added, and nitrogen gas was introduced to remove air. Then it is heated to react. The heating temperature is limited to between 120°C and 180°C depending on the solvent used. The reaction time is then set between 4 hours and 12 hours. Then stop the reaction.

[0037] 2. Vacuum distillation try to remove the solvent under reduced pressure. Add polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer in a good solvent such as dichloromethane or methanol, which is 2-8 times the amount, and stir to help dissolve it. ...

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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 specifically 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. It is widely used in various pharmaceutical dosage forms. Literature reports that polyethylene glycol monomethyl ether-dl-polylactic acid block copolymer is finally degraded 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 and certain raw materials are prepared into pharmaceutical dosage forms, they have the advantages of sustained release, targeting, safety, easy absorption, and small side effects. The methods for preparing and producing polyethylene glycol monomethyl ether-dl-polylactic acid block...

Claims

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Application Information

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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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