3,3'-Diamino-4,4'-dihydroxydiphenyl sulfone synthesis
- Product Name:3,3'-Diamino-4,4'-dihydroxydiphenyl sulfone
- CAS Number:7545-50-8
- Molecular formula:C12H12N2O4S
- Molecular Weight:280.3
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7545-50-8
The general procedure for the synthesis of bis(3-amino-4-hydroxyphenyl)sulfone from 3,3'-dinitro-4,4'-dihydroxydiphenylsulfone was as follows: 3.4 kg of 3,3'-dinitro-4,4'-dihydroxydiphenylsulfone, 9.5 kg of dimethylsulfoxide (DMSO), and 3.18 kg of aqueous 5.3% ammonium chloride were added to a reactor, and the temperature was slowly raised to 50°C. Subsequently, 2.5 kg of reduced iron powder was added in batches (material molar ratio of 3,3'-dinitro-4,4'-dihydroxydiphenylsulfone: iron: chlorinated iron). 2.5 kg of reduced iron powder was added in batches (material molar ratio of 3,3'-dinitro-4,4'-dihydroxydiphenylsulfone: iron: ammonium chloride: water: DMSO = 1:4.5:6:29:12). After completion of the reaction, hot filtration was performed and the filter cake was washed with hot DMSO. The filtrates were combined and evaporated under reduced pressure to give a mixed solution of DMSO and water, which was cooled to 5°C to promote precipitation of the product. After stopping the distillation, the solid product was collected by filtration, washed with water and dried to give 2.6 kg of 3,3'-diamino-4,4'-dihydroxydiphenyl sulfone in 93% yield.
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Yield: 98%
Reaction Conditions:
with ammonium hydroxide in 1-methyl-pyrrolidin-2-one at 150;Solvent;Temperature;
Steps:
7 Preparation of 3,3'-diamino-4,4'-dihydroxydiphenyl sulfone
To the kettle was added 40. 8 g3,3'-dibromo-4,4'-dihydroxydiphenylsulfone, 250 ml of N-methylpyrrolidone and28 g ammonia solution (molar ratio: 3, 3 '- dibromo - 4, 4' - dihydroxydiphenyl sulfone: N - methyl pyrrolidone: ammonia water = 1: 26: 8) to 150 ° C, After completion of the reaction, 160 ml of the solvent was distilled off under reduced pressure, and the remaining reaction solution was poured into water, filtered, washed with water and dried to give 27.4 g of 3,3'-diamino-4,4'-dipyldibenzene, Yield 98%.
References:
Tianjin Junkai Chemical Technology Co., Ltd.;Li, Xiaodong;Shang, Zhenhua CN105218415, 2016, A Location in patent:Paragraph 0005; 0030; 0031; 0032
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