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

Preparation method of N-alkyl phthalimide

A technology of alkyl phthalimide and phthalic anhydride, which is applied in the chemical industry, can solve problems such as residue, product loss, and yield reduction, and achieve a process with loose reaction conditions, easy realization, and simple steps Effect

Active Publication Date: 2021-03-12
JIANGMEN YOUJU NEW MATERIALS
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned existing traditional preparation methods all add organic solvents such as toluene and xylene. Although it helps the dehydration of the reaction system, the step of separating and removing the organic solvent is required in the follow-up. This process will cause product loss and reduce the yield; and the organic solvent It cannot be completely removed, and in fact there will still be residues. In addition, the use of organic solvents reduces production safety and increases production input

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
  • Preparation method of N-alkyl phthalimide
  • Preparation method of N-alkyl phthalimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Put phthalic anhydride into the flask, blow nitrogen, and slowly add dropwise an aqueous solution of isopropylamine with a molar concentration of 96%; wherein, the molar ratio of phthalic anhydride to isopropylamine is 1:3, increasing Temperature, control the temperature at 50°C, react for 2 hours, all phthalic anhydride dissolves to form a transparent solution; continue to raise the temperature to 140°C, distill out the water and excess isopropylamine in the system until there is no more water vapor in the system After the reaction is completed, the material is discharged to obtain N-isopropylphthalimide, which is a white crystal with a melting point of 81.9°C, a yield of 97%, and a purity of 99.5%.

[0039] During the distillation process, the tail gas was condensed and collected to obtain an aqueous solution of isopropylamine with a concentration of 79.6%.

Embodiment 2

[0041] Put phthalic anhydride into the flask, pass nitrogen gas, and slowly drop an aqueous solution of n-butylamine with a molar concentration of 98%; wherein, the molar ratio of phthalic anhydride to n-butylamine is 1:2; Raise the temperature, control the temperature at 90°C, react for 48 minutes, all the phthalic anhydride dissolves and form a transparent solution; continue to raise the temperature to 180°C, distill out the water and excess n-butylamine in the system until there is no more Water was evaporated, the reaction was completed, and the material was discharged to obtain N-n-butylphthalimide as white crystals with a melting point of 29.8°C, a yield of 96.2%, and a purity of 99.3%.

[0042] During the distillation process, the tail gas was condensed and collected to obtain an aqueous solution of n-butylamine with a concentration of 74.1%.

Embodiment 3

[0044] Put phthalic anhydride into the flask, pass nitrogen gas, and slowly add dropwise an aqueous solution of n-propylamine with a molar concentration of 98%; wherein, the molar ratio of phthalic anhydride to n-propylamine is 1:1.3; Temperature, control the temperature at 80°C, react for 30 minutes, all phthalic anhydride dissolves to form a transparent solution; after the dissolution is completed, transfer the material to a rotary evaporator for vacuum distillation, raise the temperature to 120°C, and distill out the system of water and excess n-propylamine, until no more water is distilled out in the system, the reaction is completed, and the material is discharged to obtain N-n-propylphthalimide, which is a white crystal with a melting point of 70.8°C and a yield of 98 %, 99.6% purity.

[0045] During the distillation process, the tail gas was condensed and collected to obtain an aqueous solution of n-propylamine with a concentration of 42%.

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

No PUM Login to View More

Abstract

The invention discloses a preparation method of N-alkyl phthalimide. The method comprises the steps: taking phthalic anhydride as a raw material, taking an aqueous solution of alkylamine as an imidization reagent ( no other reagents do not need to be added), and directly synthesizing the N-alkyl phthalimide, wherein the yield is high (96% or above), and the purity is high (99% or above). The preparation method is loose in reaction condition, simple in step and easy to implement; no organic solvent is needed, no other substances are discharged except water, and the method is green, free of pollution and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of N-alkylphthalimide. Background technique [0002] N-Alkylphthalimide is a class of important chemical raw materials, and its structure is shown in formula Ⅰ: [0003] Formula Ⅰ [0004] Wherein, R1 is a hydrogen atom or an alkyl group such as a methyl group, an ethyl group, a propyl group, an isopropyl group, a butyl group, an isobutyl group, a phenyl group, or a benzyl group. Such as N-methylphthalimide, as an important intermediate for the synthesis of drugs, pesticides, and chemiluminescent immunoassay reagents; N-ethylphthalimide, as a carrier for disperse dyes, is cited in In the printing and dyeing industry, it has the advantages of being non-toxic, improving the construction environment, and simplifying the printing and dyeing process; N-butylphthalimide is widely used as an intermediate for dyes, medicines, and spices. [0005] At p...

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
CPCC07D209/48
Inventor 王贤文胡三友张海良谭麟饶先花黄华鹏黄文刚杨思思
Owner JIANGMEN YOUJU NEW MATERIALS
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