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Process for producing 1,4-(2,4-diaminophenyloxy)-2,5-di-t-butyl benzene

A technology of diaminophenoxy and dinitrophenoxy, applied in 1 field, can solve the problems such as no patents, literature reports and the like in the preparation method, and achieve the effects of convenient source of raw materials, high yield and few chemical raw materials

Inactive Publication Date: 2008-08-20
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1,4-bis(2,4-diaminophenoxy)-2,5-di-tert-butylbenzene is an important aromatic polyvalent primary amine, but its preparation method has no patents or literature reports

Method used

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  • Process for producing 1,4-(2,4-diaminophenyloxy)-2,5-di-t-butyl benzene
  • Process for producing 1,4-(2,4-diaminophenyloxy)-2,5-di-t-butyl benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 55.4 grams (0.1 moles) of 1,4-bis(2,4-dinitrophenoxy)-2,5-di-tert-butylbenzene, 0.6 grams of palladium / carbon with a mass percentage of palladium of 15%, and 200 ml Ethanol and 670ml ethylene glycol were added in the reaction flask, stirred, heated up to 60° C., and began to add dropwise a mass concentration of 60% hydrazine hydrate solution (hydrazine hydrate molecular weight was 50.06), a total of 250.0 grams (solution weight). After the addition of hydrazine hydrate was completed, the stirring reaction was continued for 1 hour in the temperature range of 70°C to 85°C, cooled slightly, filtered while hot, cooling the mother liquor, adding pure water, and the crystalline product was precipitated, filtered, and vacuum-dried to obtain 41.0 g of 1 , 4-bis(2,4-diaminophenoxy)-2,5-di-tert-butylbenzene crystal, the purity is 99.5%, according to the actual obtained 1,4-bis(2,4-diaminophenoxy base)-2,5-di-tert-butylbenzene amount and theoretical amount (43.4 grams), calculate ...

Embodiment 2

[0029] 55.4 grams (0.1 moles) of 1,4-bis(2,4-dinitrophenoxy)-2,5-di-tert-butylbenzene, 11.0 grams of palladium mass percent is 1% palladium / carbon and 5540ml ethanol Add it into the reaction flask, stir, heat up to 60° C., and start to add dropwise a hydrazine hydrate solution with a mass concentration of 85%, totaling 294.1 grams (solution weight). After the dropwise addition of hydrazine hydrate was completed, the stirring reaction was continued for 5 hours at a temperature range of 70°C to 85°C, cooled slightly, filtered while hot, cooling the mother liquor, adding pure water, the crystallized product was precipitated, filtered, and vacuum-dried to obtain 40.6 grams of 1 , 4-bis(2,4-diaminophenoxy)-2,5-di-tert-butylbenzene crystal, the purity is 99.3%, according to the actual obtained 1,4-bis(2,4-diaminophenoxy base)-2,5-di-tert-butylbenzene amount and theoretical amount (43.4 grams), calculate 1,4-bis(2,4-diaminophenoxy)-2,5-di-tert-butylbenzene The yield was 93.5%.

Embodiment 3

[0031] 55.4 grams (0.1 mole) of 1,4-bis(2,4-dinitrophenoxy)-2,5-di-tert-butylbenzene, 4.0 grams of palladium mass percentage is 5% palladium / carbon and 1000ml 2 - Add methoxyethanol in the reaction flask, stir, heat up to 60° C., and start to add dropwise a hydrazine hydrate solution with a mass concentration of 80%, totaling 260.0 grams (solution weight). After the addition of hydrazine hydrate was completed, the stirring reaction was continued for 4 hours at a temperature range of 70°C to 85°C, cooled slightly, filtered while hot, cooling the mother liquor, adding pure water, and crystallized product was precipitated, filtered, and vacuum-dried to obtain 39.7 grams of 1 , 4-bis(2,4-diaminophenoxy)-2,5-di-tert-butylbenzene crystal, the purity is 99.4%, according to the actual obtained 1,4-bis(2,4-diaminophenoxy base)-2,5-di-tert-butylbenzene amount and theoretical amount (43.4 grams), calculate 1,4-bis(2,4-diaminophenoxy)-2,5-di-tert-butylbenzene The yield was 91.5%.

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Abstract

The invention relates to a preparation method of 1,4-double(2,4-diamino phenoxy)-2,5-d-tert-butylbenzene, comprising the steps as following, after being put into the solvent system of the solution of palladium or carbon hydrazine hydrate and saturated fatty alcohol for reaction for 1 to 5 hours with the temperature of 70 to 85 DEG C, the 1,4-double(2,4-dinitro phenoxy)-2,5-d-tert-butylbenzene is filtered when being hot, mother liquor is cooled off, pure water is dripped in, crystal products are precipitated, filtered, and dried in vacuum, and crystals of the 1,4-double(2,4-diamino phenoxy)-2,5-d-tert-butylbenzene are gained. The method has the simple operation, needs no subsequent refining and purifying technique, takes little time, has the products with the high yield and the purity of more than 99 percent, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic polyvalent primary amines, in particular to a preparation method of 1,4-bis(2,4-diaminophenoxy)-2,5-di-tert-butylbenzene. Background technique [0002] Aromatic heterocyclic polymers have excellent thermal stability, nuclear radiation resistance, flame retardancy, organic solvent resistance, and excellent high and low temperature mechanical properties and electrical properties. High-performance fields have been widely used. [0003] With the development of high-performance, lightweight, thin, and refined information electronic products, higher requirements are put forward for the insulating materials of flexible copper clad laminates (FCCL), such as high heat resistance, high strength, and low dielectric constant. and low dielectric loss etc. Therefore, polyimide materials are favored in the field of FCCL. [0004] 1,4-bis(2,4-diaminophenoxy)-2,5-di-tert-butylbenzene is one of the importa...

Claims

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Application Information

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IPC IPC(8): C07C217/90C07C213/02C07C213/00
Inventor 虞鑫海
Owner DONGHUA UNIV
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