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Preparation method for 4,4'-diamino-4''-(4-nitrophenoxy)triphenylmethane

A technology of nitrophenoxy and hydroxytriphenylmethane, which is applied in 4 fields, can solve problems such as no published literature or patent reports, and achieve the effects of easy recycling, less three wastes, and high yield

Inactive Publication Date: 2008-07-09
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] But the preparation method of 4,4'-diamino-4 "-(4-nitrophenoxy) triphenylmethane has not yet seen any published literature or patent reports

Method used

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  • Preparation method for 4,4'-diamino-4''-(4-nitrophenoxy)triphenylmethane
  • Preparation method for 4,4'-diamino-4''-(4-nitrophenoxy)triphenylmethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 29.0 grams (0.1 moles) of 4,4'-diamino-4"-hydroxytriphenylmethane, 18.9 grams (0.12 moles) of 4-chloronitrobenzene (4CNB), 24.8 grams (0.18 moles) of potassium carbonate, 252 ml N,N-dimethylformamide (DMF) and 84 milliliters of toluene were added in the round-bottomed flask with thermometer, nitrogen pipe, oil-water separator, reflux condenser and mechanical stirrer, and after nitrogen was stirred at room temperature for 0.5 hour, After heating to 100°C for 3 hours, gradually increase the reaction temperature, and finally rise to 150°C for 1 hour, and maintain the reaction at 150°C for 16 hours, then cool to 80°C, filter while it is hot, remove the filter residue, and reduce the mother liquor Concentrate under reduced pressure, cool, crystallize, filter, and dry to obtain 4,4'-diamino-4"-(4-nitrophenoxy)triphenylmethane, according to 4,4'-diamino-4"-hydroxy The feeding amount and product amount of triphenylmethane were determined, and the yield was 91% (purity 98.1%). ...

Embodiment 2

[0027] Add 29.0 g (0.1 mol) of 4,4′-diamino-4″-hydroxytriphenylmethane, 0.12 mol of potassium hydroxide, 180 ml of N-methylpyrrolidone (NMP) and 60 ml of xylene to a thermometer, nitrogen Tube, oil-water separator, reflux condenser and mechanical stirrer round-bottomed flask, after 0.5 hours of nitrogen gas stirring at room temperature, heating and reflux until no water is analyzed, cooling the reaction system to 90 ° C, adding 14.1 g (0.10 mol) 4-fluoronitrobenzene (4FNB), heating and stirring, after reacting at 120°C for 3 hours, gradually increase the reaction temperature, and finally rise to 150°C for 1 hour, and maintain the reaction at 150°C for 10 hours, then cool to 80°C, filter while hot, remove the filter residue, concentrate the mother liquor under reduced pressure, cool, crystallize, filter, and dry to obtain 4,4'-diamino-4"-(4-nitrophenoxy)triphenylmethane, according to 4,4'-diamino-4"-hydroxytriphenylmethane was measured for the amount of feed and product, and th...

Embodiment 3

[0029] 29.0 g (0.1 mol) of 4,4′-diamino-4″-hydroxytriphenylmethane, 0.12 mol of 4-bromonitrobenzene (4BNB), 0.08 mol of potassium carbonate, 120 ml of N,N-dimethylformaldehyde Amide (DMF) and 60 ml of toluene were added to a round-bottomed flask equipped with a thermometer, nitrogen tube, oil-water separator, reflux condenser and mechanical stirrer. After stirring with nitrogen at room temperature for 0.5 hours, the temperature was raised to 120 ° C for 3 hours. After that, gradually increase the reaction temperature, and finally rise to 150°C for 1 hour, and maintain the reaction at 150°C for 12 hours, then cool to 80°C, filter while it is hot, remove the filter residue, concentrate the mother liquor under reduced pressure, cool, crystallize, and filter , oven dry, obtain 4,4'-diamino-4 "-(4-nitrophenoxy) triphenylmethane, according to the charging amount and product of 4,4'-diamino-4 "-hydroxytriphenylmethane Quantitative determination, yield 68%.

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Abstract

The invention relates to a preparation process of 4, 4'- aminophenylsulfone-4''-(4- nitro phenoxy) triphenylmethane, which comprises firstly reacting 4, 4'- aminophenylsulfone-4''-hydroxy triphenylmethane and 4-halogenated nitrobenzene with molar ratio of 1:1.0-1.2 for 5-20 hours in salt forming agent, entrainer and aprotic polar solvent under nitrogen protection with 100 DEG C-150 DEG C, secondly filtering when in hot to remove filter residue, decompressing and condensing pregnant antimony solution, and then obtaining 4, 4'-aminophenylsulfone-4''-(4-nitro phenoxy) triphenylmethane through cooling, crystallization, filtration and drying. The invention has simple technology, easy recovery reaction solvent, repeated usage, less three wastes, favorable working environment and high product purity and yield, which is suitable to the industrialized production.

Description

technical field [0001] The invention belongs to the field of preparation methods of nitro-containing aromatic dibasic primary amine compounds, and in particular relates to a preparation method of 4,4'-diamino-4"-(4-nitrophenoxy)triphenylmethane. Background technique [0002] Aromatic dibasic primary amine compounds containing strong polar nitro groups in their molecular structure are important raw materials for the preparation of aromatic polyamines, and are also used for the preparation of high-temperature resistant polyimide resins, liquid crystal alignment agents, matrix resins for carbon fiber-reinforced advanced composite materials, High-impact epoxy resin curing agent, polyurethane chain extender, VLSI passivation coating and alpha particle barrier coating material, and important raw material for printed electronic circuit board substrate matrix resin or adhesive. [0003] Aromatic polyimide has excellent thermal stability, nuclear radiation resistance, excellent mecha...

Claims

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Application Information

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IPC IPC(8): C07C217/80C07C213/00
Inventor 虞鑫海
Owner DONGHUA UNIV
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