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Method for synthesizing p-hydroxystyrene by azeotropic one-pot method

A technology of p-hydroxystyrene and p-hydroxybenzaldehyde, which is applied in the field of preparation of organic compounds, can solve the problems of expensive substrate raw materials, cumbersome synthesis process, and high energy consumption, so as to simplify the material mixing process, shorten the reaction time, reduce Effects on production energy consumption and costs

Pending Publication Date: 2022-07-15
四川东材科技集团成都新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high-temperature dehydrogenation reaction method of p-hydroxyphenylethane consumes a lot of energy, and needs to add p-cresol or phenol with a substrate content of 5%-50% to participate in the reaction
In summary, the prior art preparation of p-hydroxystyrene has the disadvantages of cumbersome synthesis process, many steps, low yield, and expensive substrate raw materials

Method used

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  • Method for synthesizing p-hydroxystyrene by azeotropic one-pot method

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Experimental program
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Embodiment 1

[0026] A method for synthesizing p-hydroxystyrene by an azeotropic one-pot method, comprising the steps of: putting 50g of p-hydroxybenzaldehyde, 85g of malonic acid, 8.1g of ethylenediamine, and 0.072g of 4-tert-butylcatechol into 500ml of reaction in 45ml DMF, 135ml toluene, N 2 The reaction was carried out at 119 °C for 6 h; 300 ml of water was added, extracted and separated, washed twice with 150 ml of saturated NaCl aqueous solution, then the temperature was raised to separate the water with toluene, and the toluene was distilled off under reduced pressure to obtain a colorless oily substance, which is p-hydroxystyrene, Yield 78%.

Embodiment 2

[0028] A method for synthesizing p-hydroxystyrene by an azeotropic one-pot method, comprising the steps of: putting 50g of p-hydroxybenzaldehyde, 85g of malonic acid, 8.1g of ethylenediamine, and 0.072g of 4-tert-butylcatechol into 500ml of reaction in a container, dissolved in 60ml DMF, 120ml toluene, N 2 The reaction was carried out at 122 °C for 6 h; 300 ml of water was added, extracted, and the liquid was separated, washed twice with 150 ml of saturated NaCl aqueous solution, then the temperature was raised to toluene to separate water, and the toluene was distilled off under reduced pressure to obtain a colorless oily substance, which is p-hydroxystyrene, Yield 80%.

Embodiment 3

[0030] A method for synthesizing p-hydroxystyrene by azeotropic one-pot method, the steps are as follows: 50g p-hydroxybenzaldehyde, 85g malonic acid, 8.1g ethylenediamine, 0.1g phenothiazine are put into a 500ml reactor, dissolved In 60ml DMF, 120ml toluene, N 2 The reaction was carried out at 122 °C for 6 h; 300 ml of water was added, extracted, and the liquid was separated, washed twice with 150 ml of saturated NaCl aqueous solution, and then the temperature was increased to separate the water with toluene, and the toluene was distilled off under reduced pressure to obtain a colorless oily substance, which is p-hydroxystyrene, Yield 75%.

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Abstract

The invention discloses a method for synthesizing p-hydroxystyrene by an azeotropic one-pot method, which is characterized by comprising the following steps of: putting p-hydroxybenzaldehyde, malonic acid, a basic catalyst and a polymerization inhibitor into a reaction kettle, adding a mixed solvent of a first organic solvent and a second organic solvent to dissolve reactants, and reacting for 3-8 hours at the temperature of 105-150 DEG C in an inert gas atmosphere; and adding water into the reacted solution for washing, then adding an inorganic salt aqueous solution for washing, and then carrying out reflux water removal and reduced pressure distillation to obtain a colorless oily substance, namely the prepared p-hydroxystyrene. By adopting the method, the synthesis process is simple, the wastewater generation amount is small, the reaction temperature is low, the reaction time is short, the production energy consumption and cost are low, the yield is high, and the practicability is high, and the prepared p-hydroxystyrene is suitable for being used as a medical and chemical intermediate and is used in the fields of synthesis of medical and high polymer materials, photoresist technology and the like.

Description

technical field [0001] The invention belongs to the preparation of organic compounds, and relates to a method for synthesizing p-hydroxystyrene by an azeotropic one-pot method. The p-hydroxystyrene prepared by the invention is suitable for use as a pharmaceutical and chemical intermediate, and is used in the fields of synthesis of pharmaceuticals and polymer materials, photoresist technology and the like. Background technique [0002] p-Hydroxystyrene is an aromatic compound with wide industrial application value. It is an important pharmaceutical and chemical intermediate. It is widely used in the synthesis of medicine and polymer materials, photoresist technology and other fields. Due to the good optical properties of the polymers of p-hydroxystyrene and its derivatives, it has become the main film-forming resin material for 248nm deep ultraviolet photoresist, which is currently the mainstream photoresist product. In addition, flexible electronic devices are usually elect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/20C07C37/50C07C37/68
CPCC07C37/50C07C37/685C07C51/38C07C39/20C07C59/52
Inventor 王怡星母滨源田原周友唐安斌
Owner 四川东材科技集团成都新材料有限公司