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The preparation method of block copolymer mpeg-b-pla

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, difficulty in stable control of polymerization conditions, and low production efficiency And other issues

Active Publication Date: 2021-10-19
深圳普洛美康材料有限公司
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  • 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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  • The preparation method of block copolymer mpeg-b-pla
  • The preparation method of block copolymer mpeg-b-pla
  • The preparation method of block copolymer mpeg-b-pla

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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 preparation method of block copolymer mPEG-b-PLA. The preparation method comprises the following steps: pretreating raw materials polyethylene glycol monomethyl ether and lactide; Lactide was dissolved separately, amidine catalyst was added to polyethylene glycol monomethyl ether, lactide was added under stirring, and polymerization was carried out under anaerobic conditions for 10‑180min, and then the reaction was terminated by a terminator to obtain a crude product; the crude product was used After dissolution of the eluent, the purified product is then separated through a chromatographic column. The invention provides a method for preparing an amphiphilic block copolymer with high yield, high purity and narrow molecular weight distribution. The preparation method is solution polymerization, organic catalysis, and the reaction conditions can be precisely controlled; chromatography and centrifugation can be used for purification respectively. 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 Patents(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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