Preparation method of 4-nitrophthalonitrile

Abstract

The invention discloses a preparation method of 4-nitrophthalonitrile. The preparation method comprises the following steps: adding powdery phthalic anhydride and urea into a reaction flask, carryingout uniform mixing under stirring, carrying out a heating reaction for 0.5 hour, quickly adding water, performing stirring to allow white crystals to be precipitated, and conducting filtering and drying to obtain phthalimide; slowly adding phthalimide into a mixed solution of concentrated sulfuric acid and fuming nitric acid, carrying out uniform mixing under stirring, performing cooling in an ice-water bath, conducting a reaction for 0.5 h, carrying out heating to 60 DEG C, conducting another reaction for 3 hours, pouring a reaction product into crushed ice to obtain turbid liquid, carrying out filtering, and recrystallizing a solid by using ethanol to obtain 4-nitrophthalimide; and subjecting 4-nitrophthalimide and ammonia water with a mass fraction of 20% to mixing and ice bath treatment, carrying out filtering after a complete reaction, and carrying out washing and drying so as to obtain 4-nitrophthalonitrile. The method has the advantages of mild reaction conditions, convenient post-treatment, easy purification and high yield, and has practical application and promotion values.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, in particular to a preparation method of 4-nitrophthalonitrile. Background technique [0002] 4-Nitrophthalonitrile is a high-efficiency, low-toxic, broad-spectrum pesticide intermediate and pharmaceutical intermediate, and is also an intermediate for advanced dyes, especially for the preparation of phthalocyanine compounds, while phthalocyanine Compounds are regarded as new materials in the 21st century. The traditional synthetic route for preparing 4-nitrophthalonitrile is cumbersome, the reaction temperature is high, the raw materials used are expensive, and the purity of the obtained product is low. Contents of the invention [0003] The purpose of the present invention is to provide a method for preparing 4-nitrophthalonitrile with simple process, high yield and mild reaction conditions. [0004] The present invention comprises the following steps: (1) Add powdery phthalic anh...

AI Technical Summary

Problems solved by technology

The traditional synthetic route for preparing 4-nitrophthalonitrile is cumbersome, the reaction temperature is high, and the raw materials used are expensive, and the purity of the obtained product is low