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Crosslinked polystyrene gel and use thereof

A technology of cross-linking polystyrene and styrene, which is applied in the field of solid-phase synthesis carrier and its synthesis, can solve the problems of unsatisfactory reaction kinetics and achieve poor reaction kinetics, excellent swelling performance and chemical stability sex high effect

Inactive Publication Date: 2005-09-21
天津南开和成科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The distance between the two double bonds of this cross-linking agent is still small, and the alkane chain is in a coiled state in polar organic solvents, and the reaction kinetics of the cross-linked polystyrene carrier synthesized with it is still not ideal.

Method used

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  • Crosslinked polystyrene gel and use thereof
  • Crosslinked polystyrene gel and use thereof
  • Crosslinked polystyrene gel and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of Diethylene Glycol Dimethacrylate Crosslinked Polystyrene Gels:

[0028] Add 450ml of an aqueous solution containing 0.5% polyvinyl alcohol to a 1000ml three-necked bottle, add an organic phase solution consisting of 39.2g of styrene, 0.8g of diethylene glycol dimethacrylate and 0.2g of benzoyl peroxide, and adjust the stirring Speed, so that the diameter of the liquid droplets of the organic phase in the water phase is between 100-200 mesh, at this stirring speed, the temperature is raised to 80°C and maintained for 8 hours. The obtained bead polymer is washed several times with hot water, dried in the air, and sieved to obtain a gel of 100-200 mesh.

Embodiment 2

[0030] Preparation of Triethylene Glycol Dimethacrylate Crosslinked Polystyrene Gels:

[0031] Add 450ml of an aqueous solution containing 0.5% polyvinyl alcohol in a 1000ml three-necked bottle, add an organic phase solution composed of 38g styrene, 2g triethylene glycol dimethacrylate and 0.2g benzoyl peroxide, adjust the stirring speed, The diameter of the liquid droplets of the organic phase in the water phase is between 200-400 mesh, and the temperature is raised to 80° C. at this stirring speed and maintained for 8 hours. The obtained bead polymer is washed several times with hot water, dried in the air, and sieved to obtain a gel of 200-400 mesh.

Embodiment 3

[0033] Chloromethylation of Diethylene Glycol Dimethacrylate Crosslinked Polystyrene Gels:

[0034] Add 10g of 100-200 mesh diethylene glycol dimethacrylate cross-linked polystyrene gel (containing 3% triethylene glycol dimethacrylate, percentage by weight) into 100ml dichloromethane to swell for 1 hour , cooled to -4°C, added 10ml of chloromethyl ether, added dropwise 1.2ml of anhydrous tin tetrachloride at -4°C, and reacted at 0--4°C for 50 minutes. The resulting resin was thoroughly washed with tetrahydrofuran: 0.5mol / L HCl (volume ratio 1:1), and then fully washed with tetrahydrofuran and distilled water until the resin was washed with AgNO 3 The absence of chloride ions was detected and the resulting resin was vacuum dried. The chlorine content of the obtained resin was measured to be 1.32 mmol / g.

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Abstract

The invention relates to a new crosslinked polystyrene gel and its application. In the invention, combining the dimethacrylic acid diglycol ester or dimethacrylic acid diglycol ester as cross linking agents with phenylethene or phenylethene substitution copolymer gel to get the product by free radical copolymerization. The gel with functional group can be used as a solid phase carrier of solid phase method of polypeptide synthesis, solid phase organic synthesis or combination chemical as well as a solid phase scavenging agent.

Description

【Technical field】 [0001] The invention relates to a solid-phase synthesis carrier and a synthesis method thereof, in particular to a new type of cross-linked polystyrene gel and its application. 【Background technique】 [0002] In 1963, Merrifield invented the solid-phase peptide synthesis method (R.B.Merrifield, J.Am.Chem.Soc., 1963, 85, 2149). Since then, the solid-phase synthesis method has been widely used in solid-phase peptide synthesis, solid-phase organic synthesis and combinatorial chemistry middle. The advantages of solid-phase synthesis include: (1) Excess reagents can be used to complete the reaction. (2) The product of each step is immobilized on a solid phase carrier insoluble in any solvent, so the separation of the desired product from other small molecule reagents such as excess reagents and catalysts can be achieved by simple filtration. (3) In all the operation steps before lysis, the solid phase carrier is always in the same container without any mechani...

Claims

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Application Information

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IPC IPC(8): C08F2/00C08F257/02
Inventor 阎虎生马玉新王玉史作清路延龄张更辉范云鸽孙强姜文花
Owner 天津南开和成科技有限公司