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ChemicalBook CAS DataBase List 4-PHENYLAZOPHENOL

4-PHENYLAZOPHENOL synthesis

9synthesis methods
aniline diazotization, and phenol coupling.
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Yield:1689-82-3 97%

Reaction Conditions:

Stage #1:aniline with potassium bisulfite;sulfuric acid in water at 8 - 9;
Stage #2:phenol with potassium carbonate in water; pH=3-9 for 0.833333 h;Temperature;

Steps:

3 Example 3:
(i) in the presence of a stirrer,A thermometer and a dropping funnel, 300 ml of a sulfuric acid solution having a mass fraction of 10%The stirring speed was controlled at 200 rpm,Slowly add aniline 1.2mol, completely dissolved after reducing the solution temperature to 9 ,Dropping potassium hydrogen sulfite 1.1mol dissolved in 230ml water dubbed solution,The solution temperature was controlled at 8 ° C and the reaction end point was determined by potassium iodide paper to form diazonium salt (3).
(ii) 2.3 L of a 9% potassium carbonate solution in a separate container,Phenol 1.2 mol,Dubbed phenol potassium solution,The diazotized solution obtained in step (i) was slowly added at a stirring speed of 160 rpm,The pH value of the solution was kept at 9, then the pH was lowered to 3 by adding oxalic acid solution, the reaction was maintained for 50 min, filtered, and the sodium bicarbonate washing solution was added, and no solution was added, and the solution was kept at the temperature of 20 DEG C. Sodium sulfate dehydration, 4-hydroxy azobenzene (1) 230.47g, the yield of 97%.

References:

Chengdu Zhongheng Huatie Technology Co., Ltd.;Peng, Xiangliang CN105601534, 2016, A Location in patent:Paragraph 0018; 0019; 0020

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