The invention provides a preparation technique of p-acetaminophenoxide; the technique includes the following steps: adding
phenol, oxammonium
hydrochloride,
acetic acid and
polyphosphate with
mass ratio of 1 : 0.85 : 3.0 : 8.5 to 1 : 0.96 : 4.1 : 9.6 into a reactor and sealing the reactor; carrying out
reflux reaction for 3.0 to 5.2h under normal pressure and constant temperature in an
oil bath of 75 to 85 DEG C; cooling to the temperature of 20 to 30 DEG C; adding
ice water of 10 to 15 times of the volume of the mixed matters into the reactor and adjusting pH to 3.5 to 4.5 by using
ammonia; adding
nitrogen into the reactor to replace air; adding
sodium bisulfite of 1 to 2 times of the weight of
phenol and then sealing the reactor, continuously carrying out reaction for 5.0 to 7.2h under the normal pressure and constant temperature in the
oil bath of 110 to 132 DEG C, cooling, decompressing and vaporizing the
solvent water, then using
acetone to wash so as to filter out
ammonium phosphate salt,
combing the filtrate, vaporizing and recycling the
acetone to obtain the crude product, using water to re-crystallize to obtain the white
crystal of the p-acetaminophenoxide. The preparation technique of the invention takes the
phenol, glacial
acetic acid and the oxammonium
hydrochloride as the raw materials, takes the
polyphosphate as a catalyst, adopts one pot method to prepare the p-acetaminophenoxide and has the advantages of simple technique, mild
reaction conditions, low manufacture cost and being environment friendly.