4,4'-dimercaprol azobenzene and preparation method thereof

2010 
4,4-dimercapto-azobenzene and its preparation method, azo relates to a mercapto compound. 4,4-dimercapto-azobenzene formula HS (C6H4) N = N (C6H4) SH. After the aniline was dissolved in aqueous sodium bicarbonate, I2 was added after the reaction, the solvent was drained under reduced pressure to give 4-iodo-aniline, and then dissolved in glacial acetic acid was added NaBO3 · 4H2O and H3BO3 reaction, with THF Recrystallization from 4,4 '- diiodo after azobenzene, dissolved in THF, was added portionwise magnesium turnings reacted azobenzene was cooled to give a Grignard reagent; sulfur powder was added to the solid azobenzene Grignard reagent, the reaction was heated after vulcanized product, after cooling, NH4Cl solution, and then acidified with hydrochloric acid and extracted with dichloromethane, the organic phases were combined, dried filtered and the solvent was distilled off under reduced pressure and the crude product was extracted with ethanol, the solvent was evaporated to dryness to give the product.
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