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Synthesis method of diene crosslinking agent 1,4-di(4'- vinyl phenoxy) butane

A technology of ethylene phenoxy and synthesis method, which is applied in ether preparation, organic chemistry, etc., can solve the problems of high synthesis cost, inconvenient storage, transportation, and high price, and achieve the effects of simple operation, easy separation and purification, and low cost

Inactive Publication Date: 2006-01-04
NANKAI UNIV
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  • Abstract
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Problems solved by technology

However, the price of p-acetoxystyrene is relatively high, and there is no such raw material produced in China at present, and p-acetoxystyrene is a liquid containing ethylenic bonds, which is prone to polymerization, which causes inconvenience to storage and transportation, so 1,4- The synthesis cost of bis(4'-vinylphenoxy)butane is relatively high

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  • Synthesis method of diene crosslinking agent 1,4-di(4'- vinyl phenoxy) butane
  • Synthesis method of diene crosslinking agent 1,4-di(4'- vinyl phenoxy) butane
  • Synthesis method of diene crosslinking agent 1,4-di(4'- vinyl phenoxy) butane

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Embodiment Construction

[0009] The present invention will be described in detail below in conjunction with examples.

[0010] Diene crosslinking agent 1 of the present invention, the synthetic method of 4-bis (4 '-vinylphenoxy) butane, take p-hydroxyacetophenone as raw material, through etherification with 1,4-dibromobutane, the Carbonyl reduction, dehydration into alkene, to obtain this diene crosslinking agent, wherein:

[0011] Compound (I) is generated by adding p-hydroxyacetophenone and 1,4-dibromobutane in the presence of a base, adding an organic solvent, stirring and reacting at reflux temperature for 8-16 hours. Said alkali can be: one or more mixtures in sodium carbonate, potassium carbonate or sodium methylate. Said organic solvent can be: one or more mixtures in acetonitrile, propanol or isopropanol.

[0012] Then, compound (I) is reacted with stirring reaction for 6-10 hours at 45-50° C. with 1.2-2.0 mole ratio of (I) reducing agent in 1:1 tetrahydrofuran:ethanol solvent to obtain inte...

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Abstract

A process for synthesizing the diene cross-linking agent 1,4-bis (4'-vinylphenoxyly) butane from p-hydroxy acetophenone includes such steps as etherifying with 1,4-dibromobutane, reduction and dewatering.

Description

【Technical field】 [0001] The invention relates to a synthesis method of a high-molecular polymer monomer, in particular to a synthesis method of a diene crosslinking agent 1,4-bis(4'-ethylenephenoxy)butane. 【Background technique】 [0002] 1,4-bis(4′-ethylenephenoxy)butane is also known as Janda Linker; as early as 1987, J.Ericcson et al. (See Ericcson J.and Hult A., Polym.Bull., 1987, 18:295) Using p-hydroxybenzaldehyde as the starting material, this monomer was synthesized after introducing ethylenic bonds through Wittig reaction and then reacting with 1,4-dibromobutane. It is mainly used for cationic polymerization to study cationic polymerization with better mechanical properties thing. Janda and colleagues (see Toy P H, Janda K D, Tetrahedron Lett, 1999, 40: 6329 and Toy P H, Reger T S, Garibay P, et al, J Comb Chem, 2001, 3: 117] used this monomer as a The polystyrene-type solid-phase carrier resin was prepared by using a coupling agent. This kind of carrier resin usi...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/243C07C41/01
Inventor 范云鸽史作清施荣富路延龄
Owner NANKAI UNIV