| 摘要 |
Oxyphenbutazone drugintermediates 4-hydroxyazobenzene synthesis method, comprising the following steps: equipped with a stirrer, a thermometer and a dropping funnel, a reaction vessel was added 300ml a certain concentration of sulfuric acid solution, stirring rate was controlled at 100-200 rpm, 1.2 mol aniline was added slowly, after complete dissolution the solution is reduced to a temperature of 6-9 C, 1.Imol potassium bisulfate was added dropwise in 200-230ml aqueous solution, during dissolution process the temperature was controlled at 6-8 'C, KI test paper measuring the end of the reaction, generating diazonium salt solution; adding 2-2.31 a certain concentration of potassium carbonate solution in another vessel, 1.2mol phenol, formed potassium phenol solution, diazonium salt solution was added slowly under a stirring rate of 100-160rpm,the temperature of the solution is controlled at 16-20 C, after the addition the reaction continued for another 30-40min, the regulating solution was added, the pH of the solution is maintained at 8-9, and then oxalic acid solution was added to reduce the pH to 2-3, maintain the reaction for 40-50min, filtration, added to the washing solution, dehydrated with dehydrating agent, ultimately got 4-hydroxyazobenzene. |
