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Synthetic technology of p-methoxystyrene

A technology of methoxystyrene and a synthesis process, applied in the chemical field, can solve problems such as long reaction period, unfavorable industrial continuous production, etc., and achieve the effects of low production cost, little environmental pollution, and reduced production cost

Inactive Publication Date: 2010-06-23
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above two process routes have a long reaction cycle, which is not conducive to continuous industrial production; with the one-pot method, the generated p-methoxystyrene is easy to polymerize in the flask

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The concrete processing step of the inventive method is described as follows now:

[0025] a. Add 500g of p-methoxyacetophenone, 150ml of ethanol and 150ml of water to a three-necked flask equipped with mechanical stirring and a serpentine condenser, raise the temperature to 80°C, add 52g of potassium borohydride in batches within 30min, and react 4 Hour. Add 300ml of water to wash off the excess potassium borohydride, let stand to separate the liquid to remove the water layer, add anhydrous magnesium sulfate to remove the residual water, and use a rotary evaporator to evaporate the ethanol under reduced pressure to obtain compound I, which is p-methoxy-α-formazol 490.5g of benzyl alcohol. The yield is 96.8%, and the content detected by GC is 99.5%.

[0026] b. Add 12.5 g of p-methoxy-α-methylbenzyl alcohol and 0.52 g of potassium bisulfate to a three-necked flask equipped with mechanical stirring, raise the temperature to 60° C., and stir for 2.5 hours. Unreacted po...

Embodiment 2

[0029] This example is basically the same as Example 1, except that in step a, the temperature is 65° C., and the reaction time is 6 hours. 493.8 g of p-methoxy-α-methylbenzyl alcohol was obtained. The yield is 97.3%, and the content detected by GC is 99.1%.

Embodiment 3

[0031] This embodiment is basically the same as Embodiment 1, except that in step a, the solvent alcohol used is propanol, 150ml of propanol and water. 490 g of p-methoxy-α-methylbenzyl alcohol was obtained. The content detected by GC was 99.0%, and the yield was 95.7%.

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Abstract

The invention relates to a synthetic technology of p-methoxystyrene, which comprises: using p-methoxyhypnone as a raw material, reducing to p-methoxy-alpha-methylbenzylalcohol by a reducing agent, adding a small quantity of weakly acidic catalyst to the p-methoxy-alpha-methylbenzylalcohol, agitating and reacting for a period of time, taking liquid, and flowing the liquid through a tubular reactor under negative pressure to generate the p-methoxystyrene, wherein the tubular reactor is used for replacing the reactor units such as traditional reaction kettles and the like, continuous production can be conveniently carried out and production cost is greatly decreased.

Description

technical field [0001] The invention relates to a synthesis process of p-methoxystyrene, which belongs to the technical field of chemical industry. Background technique [0002] p-methoxystyrene, structural formula (IV) [0003] [0004] Styrenic compounds are important monomers for the synthesis of polystyrene resins. Various substituents on the benzene ring can endow the prepared polystyrene resins with various properties and be used in various places. The polymer of p-methoxystyrene is an excellent anti-corrosion material and is widely used in the information industry. There are many reports on its synthetic methods in the literature, and the specific synthetic methods are: [0005] US005489731A utilizes Wittig reaction, takes p-methoxybenzyl alcohol as raw material to react with triphenylphosphine, formaldehyde, hydrobromic acid to prepare p-methoxystyrene. The price of raw materials used in this route is high, and the post-treatment process is complicated. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/215C07C41/18B01J14/00
Inventor 杨晖蒋茹强左翔
Owner NANJING TECH UNIV
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