Perfume fouramine and derivant thereof and preparation method and application thereof
A reaction and action technology, applied in the field of aromatic tetraamine and its derivatives, can solve the problems of high dielectric constant, poor solubility, limited types of aromatic tetraamine compounds, etc., and achieve high yield, mild reaction conditions, excellent The effect of alkali resistance or solubility
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Embodiment 1、1
[0051] Embodiment 1,1, the synthesis of 4-two (3 ', 4'-diaminophenoxy) benzene
[0052] With 34.5 grams (0.20mol) 5-chloro-2-nitroaniline (R in formula III 1 stands for Cl, R 2 stands for NO 2 ), 11 grams of hydroquinone (0.10mol), 55.2 grams of anhydrous potassium carbonate (0.40mol) and 300ml N,N-dimethylformamide were put into a 1000mL three-necked reaction flask and stirred to mix evenly. The reaction flask was heated to 100° C., and the reaction was stirred for 24 hours under nitrogen. After cooling to room temperature, the reaction solution was poured into 1000 ml of cold water with stirring. Filtrate, collect the precipitate, wash repeatedly with deionized water, then dry under vacuum at 110°C, and finally recrystallize with ethanol to obtain 34.4 grams of 1,4-bis(3'-amino-4'-nitrophenoxy )benzene.
[0053] 38.2 grams of 1,4-bis(3'-amino-4'-nitrophenoxy)benzene prepared above were completely dissolved in 400 ml of ethanol, and 1.8 grams of 5% palladium / carbon catal...
Embodiment 2、1
[0060] Embodiment 2,1, the synthesis of 3-bis(3', 4'-diaminophenoxy group) benzene
[0061] 70.3 grams (0.45mol) of 5-fluoro-2-nitroaniline (R in the formula III 1 stands for F, R 2 stands for NO 2 ), 22 grams (0.20mol) of resorcinol, 63.6 grams of anhydrous sodium carbonate (0.60mol) and 400ml of dimethyl sulfoxide were put into a 1000mL three-necked reaction flask and stirred evenly. The reaction flask was heated to 180° C., and the reaction was stirred for 1 hour under nitrogen. After cooling to room temperature, the reaction solution was poured into 1500 ml of cold water with stirring. Filtrate, collect the precipitate, wash repeatedly with deionized water, then dry under vacuum at 110°C, and finally recrystallize with ethanol to obtain 69.5 grams of 1,3-bis(3'-amino-4'-nitrophenoxy )benzene.
[0062] 57.3 grams of 1,3-bis(3'-amino-4'-nitrophenoxy)benzene prepared above were completely dissolved in 500 ml of ethanol, and 1.8 grams of 5% palladium / carbon catalyst was a...
Embodiment 3、1
[0069] Embodiment 3,1, the synthesis of 2-two (3 ', 4'-diaminophenoxy) benzene
[0070] Put 43.1 grams (0.25mol) of 5-chloro-2-nitroaniline, 11 grams (0.10mol) of catechol, 27.6 grams of anhydrous cesium carbonate (0.20mol) and 300ml of dimethyl sulfoxide into 1000mL three-port reaction Stir in the bottle to mix well. The reaction flask was heated to 80° C., and the reaction was stirred for 72 hours under nitrogen. After cooling to room temperature, the reaction solution was poured into 1000 ml of cold water with stirring. Filtrate, collect the precipitate, wash repeatedly with deionized water, then dry under vacuum at 110°C, and finally recrystallize with ethanol to obtain 34.0 g of 1,2-bis(3'-amino-4'-nitrophenoxy )benzene.
[0071] 38.2 grams of 1,2-bis(3'-amino-4'-nitrophenoxy)benzene prepared above were completely dissolved in 400 ml of ethanol, and 2.0 grams of 5% palladium / carbon catalyst was added. After the reaction flask was heated to reflux, 110 ml of hydrazine ...
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