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3-(Diphenylamino)phenol synthesis

10synthesis methods
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Yield: 59%

Reaction Conditions:

with tri-tert-butyl phosphine;o-xylene;palladium diacetate;sodium t-butanolate in chloroform at 120; for 8 h;Inert atmosphere;

Steps:

2 EHTPA Synthesis
In a nitrogen stream, sodium 3-amino benzoic acid (llg, 100mmol), bromobenzene (31g, 200mmol), t-butanol(38g, 400mmol), tri-t-butylphosphine (0. 40g, 2. OOmmol) and palladium acetate (0. 45g, 2. OOmmol) were added to xyleneThe (250g), was stirred at 120 ° C for 8 hours. Chloroform was added to the reaction solution (1.0L), with a 10 wt% aqueous ammonium chlorideThe solution (500mLX2) cleaning, washed with water (500mLX2). Dried over magnesium sulfate, and purified by column chromatography (baby gum, n-hexyl burn/ Chloroform = 1/1 (ν / ν)) to give a gray powder of the compound 1 (15. 5g, 59% yield).

References:

National University Corporation,Kyushu University;Nissan Chemical Industries, Ltd;ADACHI, CHIHAYA;XU, DENGHUI;HIRATA, SHUZO;HIRATA, OSAMU;SHIBANO, YUKI CN102473853, 2016, B Location in patent:Paragraph 0222-0224