Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Prepn process of N-methyl-4-(dimethyl phenoxy) phthalimide

A technology of dimethylphenoxy and nitrophthalimide, which is applied in the field of preparation of N-methyl-4-phthalimide, can solve the problems of low product yield, three wastes treatment, cumbersome operation process, etc.

Active Publication Date: 2005-12-14
SHANGHAI PLASTICS RES INST CO LTD
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The operation process of the prior art is cumbersome, and anhydrous potassium carbonate and other reactants are not added to the reactor at one time; the reaction product is stirred and precipitated in dilute hydrochloric acid, which brings the problem of three wastes treatment; N-methyl-3-chloro Substituted phthalimide as raw material product yield is low

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Prepn process of N-methyl-4-(dimethyl phenoxy) phthalimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 680ml of DMAC, 70 grams of 2,3-dimethylphenol, 115 grams of N-methyl-4-nitrophthaloyl in a 1000ml three-necked flask equipped with a stirrer, reflux condenser, inert gas inlet and outlet tubes, and a thermometer. Amine, 44 grams of anhydrous potassium carbonate, 5.4 grams of tetrabutylammonium bromide, under a nitrogen atmosphere, heat and stir to dissolve the solid, raise the temperature to 132 ° C, keep the temperature for 12 hours, and filter the reaction solution while it is hot when the reaction is over , cooling the filtrate to room temperature, standing overnight, and filtering the precipitate to obtain 153.4 grams of N-methyl-4-(2,3-dimethylphenoxy)phthalimide solid crystal product, the color is light yellow, The melting point is 162-163.5°C, and the yield is 94%.

Embodiment 2

[0020] In addition to adding 606ml of DMAC, 120 grams of N-methyl-4-nitrophthalimide, 50 grams of anhydrous potassium carbonate, and 12.6 grams of tetrabutylammonium bromide, and raising the temperature to 131 ° C, other process steps and material ratios And reaction parameters are all identical with embodiment 1, the result obtains 151.5 grams of N-methyl-4-(2,3-dimethylphenoxy) phthalimide light yellow crystalline powder product, fusing point 163~164.5 ℃, obtains The rate is 93%.

Embodiment 3

[0022] Except for adding 2.4 grams of tetrabutylphosphorus bromide and raising the temperature to 135°C, other process steps, material proportions and reaction parameters were the same as in Example 1, resulting in 150.1 grams of N-methyl-4-(2,3- Dimethylphenoxy)phthalimide is a light yellow crystalline powder product with a melting point of 163-165°C and a yield of 92%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Melting pointaaaaaaaaaa
Melting pointaaaaaaaaaa
Login to View More

Abstract

In the presence of tetrabutyl bromide and inside N, N-dimethyl acetylamide, dimethyl phenol, N-methyl-4-nitro phthalimide and anhydride alkali metal carbonate react at 130-135 deg.c for 12 hr; the reacted solution is filtered while being hot; the filtrate is cooled to room temperature to separate out crystal; and through filtering, yellowish solid crystal N-methyl-4-(dimethyl phenoxy) phthalimide is obtained in the yield of 92-95 %. The product of the present invention is the intermediate product of ODPA as the important polyimide.

Description

technical field [0001] The present invention relates to the preparation method of N-methyl-4-(dimethylphenoxy) phthalimide, more precisely the present invention relates to dimethylphenol and N-methyl-4-nitrophthalimide A method for preparing N-methyl-4-(dimethylphenoxy)phthalimide by amine reaction. Background technique [0002] It is well known that polyimide has excellent thermal stability and mechanical properties at high temperature. Due to its insoluble and infusible properties, it is difficult to process, which limits its use. In order to improve the processing performance of polyimide, many scholars have done extensive research, and the more convenient method is to synthesize isomerized polyimide by using isomeric monomers. Polyimide with asymmetric molecular structure shows better solubility and melt processing performance. This theory is more and more accepted by polyimide workers. Prior art, Journal of Polymer Science Part A: Polymer Chemistry, 2003, 41[21]: 324...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D209/48
Inventor 吕凯华向阳胡志强
Owner SHANGHAI PLASTICS RES INST CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com