The invention discloses a synthetic method for an oxyphenbutazone
drug intermediate-4-hydroxyazobenzene. The method comprises the following steps: (i) adding 300ml of a
sulfuric acid solution with a certain concentration into a reaction container equipped with a stirrer, a temperature meter and a drop funnel, controlling the stirring speed to be 100-200rpm, slowly adding 1.2mol of phenylamine, after phenylamine is completely dissolved, cooling the solution to 6-9 DEG C, dropwise adding 1.1mol of
potassium bisulfite, performing
dissolution in 200-230ml of water to prepare a solution, testing a reaction termination point by using
potassium iodide test paper, and generating diazonium salt (3); and (ii) adding 2-2.3L of a
potassium carbonate solution with a certain concentration and 1.2mol of
phenol into the other container to prepare a potassium phenate solution, slowly adding a diazotization solution obtained in the step (i) at the stirring speed of 100-160rpm, controlling the temperature of the solution to be 16-20 DEG C, after the addition is finished, continuing to react for 30-40 minutes, adding an adjusting solution for maintaining the pH value of the solution to be 8-9, then adding an
oxalic acid solution for reducing the pH value to be 2-3, keeping the reaction for 40-50 minutes, performing suction
filtration, adding a washing solution, and performing
dewatering with a
dewatering agent to obtain 4-hydroxyazobenzene.