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Bi(N-methylphthalic imidine) ester preparation method

A technology of methyl phthalimide and nitro phthalimide, applied in the field of bis-ether preparation, can solve problems such as high cost, difficulty in popularization and application, and large amount of three wastes to be treated, and achieves The effect of low production cost, easy recycling and low environmental pollution

Inactive Publication Date: 2009-02-11
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, existing method produces two (N-methylphthalimide) ether product cost heights, and the three wastes treatment amount is big, is difficult to popularize and apply

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 206 grams (1mol) N-methyl-4-nitrophthalimide and composite catalyst in 1000ml (three-necked flask) equipped with stirrer, condenser, thermometer: 63.6 grams (0.6mol) sodium carbonate , 16.2 grams (0.27mol) of fumed white carbon black, 8.05 grams (0.025mol) of tetrabutylammonium bromide and 270ml dimethyl sulfoxide, heated and stirred to reflux, and after 6 hours, the reaction ended, filtered while hot, and the filtrate was cooled After reaching room temperature, the product precipitated. After filtering, recovering the solvent, washing with water and drying, 127 grams of brown-yellow bis(N-methylphthalimide) ether product was obtained, with a yield of 75.6% and a melting point of 268.5 to 271°C

Embodiment 2

[0017] With embodiment 1, add composite catalyst and be: 74.2 grams (0.7mol) sodium carbonate, gas-phase white carbon black 14.7 grams (0.245mol), tetrabutylammonium bromide 14.49 grams (0.045mol) react 8 hours. Other conditions are identical with embodiment 1. 133 g of brown-yellow bis(N-methylphthalimide) ether was obtained with a yield of 79.2% and a melting point of 269-271°C.

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Abstract

The invention discloses a making method of di (N-methyl phthaloyl imine) ether, which comprises the following steps: proceeding self-condensing reaction for N-4-nitro phthaloyl imine in the polar non-proton solvent under composite catalyst and normal pressure; heating to reflux 6-8h; filtering; cooling; evolving product; washing; drying to recycle solvent; obtaining the composite catalyst with gas-phased silica, sodium carbonate and phase-transmitting catalyst.

Description

technical field [0001] The present invention relates to a heterocyclic compound having oxygen atoms at positions 1 and 3, and more specifically relates to a preparation method of bis(N-methylphthalimide) ether. Background technique [0002] ODPA is one of the important monomers for the preparation of high temperature resistant resins such as meltable polyimides, and bis(N-methylphthalimide) ether is used to synthesize 3,3',4,4'-diphenyl The intermediate of ether tetracarboxylic dianhydride, with the continuous development of new polyimide materials in my country, ODPA has been paid more and more attention as a key new material monomer. Bis(N-methylphthalimide) ether The demand is also increasing year by year. At present, the preparation method of two (N-methylphthalimide) ethers is mainly to carry out self-condensation with nitrites of alkali metals and alkaline earth metals or with catalyzers such as potassium fluoride and sodium fluoride. The yield of -methylphthalimide) e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48
Inventor 黄英
Owner SHANGHAI INST OF TECH
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