Method for preparing p-acetoxystyrene by one-pot method

Abstract

The method is characterized by comprising the following steps: putting p-hydroxybenzaldehyde, malonic acid, a basic catalyst and a polymerization inhibitor into a reaction kettle, adding an aprotic polar solvent or a mixed solvent of the aprotic polar solvent and toluene to dissolve reactants, and reacting at the temperature of 60-80 DEG C in an inert gas atmosphere to obtain p-acetoxystyrene; reacting at the temperature of 105-150 DEG C for 5-8 hours to obtain a reacted solution; and adding an extracting agent into the solution after the reaction, stirring, then adding an acetylation reagent and alkali, reacting for 4-6 hours at the temperature of 30-50 DEG C, and then performing post-treatment to obtain p-acetoxystyrene. By adopting the method, only two-step reaction is needed, the two-step reaction can be carried out in one pot, the reaction steps are few, the operation is simple, the reaction condition is mild, the equipment requirement is low, the comprehensive cost is low, and the practicability is high; the prepared p-acetoxystyrene is suitable for being used as a medical and chemical intermediate.

Description

technical field [0001] The invention belongs to the preparation of organic compounds, and relates to a one-pot method for preparing p-acetoxystyrene. The p-acetoxystyrene prepared by the invention is suitable for use as pharmaceutical and chemical intermediates, especially for photoresist intermediates in the microelectronics industry, and can also be used for elastomers, resins, coatings, adhesives, inks, and automotive surfaces. Preparation of paint, etc. Background technique [0002] As an important aromatic compound, p-acetoxystyrene is an important intermediate for the synthesis of 248nm deep ultraviolet positive photoresist and one of the important raw materials for photoresist. It is of great significance to the development of the microelectronics industry at home and abroad. In addition, p-acetoxystyrene can be used in the preparation of elastomers, resins, coatings, adhesives, inks, automotive topcoats, etc., so it has broad market prospects. [0003] In the prio...

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Problems solved by technology

However, expensive Green's reagent and Wittig's reagent are used here, and the requirements for equipment and operation are very high, and the yield of the product is low, only 12% to 42%.

In addition, p-ethylphenol is used as a raw material to synthesize p-hydroxystyrene by catalytic dehydrogenation, and then esterified to obtain p-acetoxystyrene. Although this type of method has good selectivity, catalytic dehydrogenation requires Carried out under gas phase conditions, the requirements for reaction temperature and equipment are relatively high, which is not conducive to large-scale industrial production

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