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Block copolymer mPEG-b-PLA preparation method

A block copolymer, mpeg-b-pla technology, applied in the field of block copolymer mPEG-b-PLA preparation, can solve the problem of difficult control of product molecular weight and molecular weight distribution, low production efficiency, and difficult to stably control polymerization conditions And other issues

Active Publication Date: 2019-10-22
深圳普洛美康材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the synthesis reaction of this block polymer is ring-opening polymerization, the common method in the prior art is bulk polymerization, but bulk polymerization requires high temperature, and the reaction time usually needs more than 12h. The polymerization conditions are difficult to control stably, and the production efficiency is low. and the molecular weight distribution is difficult to control

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  • Block copolymer mPEG-b-PLA preparation method
  • Block copolymer mPEG-b-PLA preparation method
  • Block copolymer mPEG-b-PLA preparation method

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preparation example Construction

[0036] A preparation method of block copolymer mPEG-b-PLA, comprising the following steps:

[0037] (1) Raw material processing: Weigh polyethylene glycol monomethyl ether and lactide, dissolve polyethylene glycol monomethyl ether in a volatile organic solvent, remove water, filter for later use; recrystallize lactide, and dry Standby; Wherein, polyethylene glycol monomethyl ether: the weight ratio of lactide is (0.1~30): 1; Described volatile organic solvent selects the alkane of low carbon chain or substituted alkane, and described carbon chain length is C 1 -C 10 .

[0038] (2) Synthesis of mPEG-b-PLA: polyethylene glycol monomethyl ether and lactide are dissolved with volatile organic solvents respectively to obtain polyethylene glycol monomethyl ether solution and lactide solution. The preferred low-carbon chain alkane or substituted alkane of the organic solvent, the carbon chain length is C 1 -C 10 . Next, add amidine catalyst to the polyethylene glycol monomethyl ...

Embodiment 1

[0044] Embodiment 1, a kind of preparation method of block copolymer mPEG-b-PLA (mPEG1000-b-PLA9000), comprises the following steps:

[0045] (1) Raw material treatment: take polyethylene glycol monomethyl ether (PEG1000) and lactide as raw materials, dissolve polyethylene glycol monomethyl ether in dichloromethane, remove water with molecular sieves, and filter for later use; The ester was recrystallized twice with ethanol and dried for later use;

[0046] (2) Synthesis of mPEG-b-PLA: Dissolve pretreated 1g mPEG1000 in 50mL dichloromethane, stir at 500r / min to obtain mPEG1000 solution, add 240μL DBN; dissolve 9g lactide in 50mL dichloromethane to obtain lactide solution, and then the lactide solution was transferred to the mPEG1000 solution, the air was removed, and the vacuum degree was 0.1Mpa. After reacting for 180 minutes, 110 μl of glacial acetic acid was added to terminate the reaction, and the stirring was continued for 10 minutes. The crude product was obtained after ...

Embodiment 2

[0049] Embodiment 2, a kind of preparation method of block copolymer mPEG-b-PLA (mPEG1000-b-PLA3000), comprises the following steps:

[0050] (1) Raw material treatment: take polyethylene glycol monomethyl ether (PEG1000) and lactide as raw materials, dissolve polyethylene glycol monomethyl ether in dichloromethane, remove water with molecular sieves, and filter for later use; The ester was recrystallized twice with ethanol and dried for later use, wherein the weight ratio of polyethylene glycol monomethyl ether: lactide was 1:3.

[0051] (2) Synthesis of mPEG-b-PLA: pretreated 2g mPEG1000 was dissolved in 50mL dichloromethane, stirred at 500r / min to obtain mPEG1000 solution, 130μg TBD was added; 6g lactide was dissolved in 50mL dichloromethane to obtain lactide solution, and then the lactide solution was transferred to the mPEG1000 solution, the air was removed, and the vacuum degree was 0.09Mpa to react for 30 minutes; 89 μg of benzoic acid was added to terminate the reactio...

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Abstract

The invention discloses a block copolymer mPEG-b-PLA preparation method, which comprises: pre-treating raw materials polyethylene glycol monomethyl ether and lactide; respectively dissolving the polyethylene glycol monomethyl ether and the lactide; adding an amidine-based catalyst to the polyethylene glycol monomethyl ether, adding the lactide under stirring, polymerizing for 10-180 min under anaerobic conditions, and terminating the reaction by using a terminating agent to obtain a crude product; and dissolving the crude product with an eluant, and separating by a chromatography column to obtain a purified product. According to the present invention, the preparation method of the amphiphilic block copolymer with characteristics of high yield, high purity and narrow molecular weight distribution is provided, uses solution polymerization and organic catalysis, can precisely control the reaction conditions, and can perform purification respectively through chromatography and centrifugation, and the molecular weight dispersion of the obtained block copolymer can be controlled within 1.1.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and relates to a synthesis and purification method of a block copolymer, in particular to a preparation method of a block copolymer mPEG-b-PLA. Background technique [0002] The block copolymer mPEG-b-PLA is a good carrier of therapeutic drugs, which can increase the solubility of poorly soluble drugs such as anticancer drugs and reduce the side effects of drugs. Because the synthesis reaction of this block polymer is ring-opening polymerization, the common method in the prior art is bulk polymerization, but bulk polymerization requires high temperature, and the reaction time usually needs more than 12h. The polymerization conditions are difficult to control stably, and the production efficiency is low. And the molecular weight distribution is difficult to control. Contents of the invention [0003] The technical problem to be solved in the present invention is to provide a prepara...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/664C08G63/87C08G63/90
CPCC08G63/664C08G63/823C08G63/90
Inventor 唐键胡霏
Owner 深圳普洛美康材料有限公司
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