Belonging to the technical field of
phenothiazine derivative synthesis, the invention relates to a synthesis method of high purity dioxopromethazine
hydrochloride, which comprises: adding
toluene and dioxophenothiazine into a reaction kettle, stirring, adding a
sodium hydroxide solid and a 2-chloro-N, N-dimethyl-1-
propylamine toluene solution, carrying out heating
reflux reaction, liquid separation, washing, concentration, adding a
solvent, heating, adding an acid to adjust the pH value, and cooling to
room temperature to obtain the high purity dioxopromethazine
hydrochloride. Stirring, cooling and crystallizing, filtering and
drying to obtain dioxopromethazine
oxalate; the preparation method comprises the following steps: adding
toluene and
purified water into a reaction kettle, adding dioxopromethazine
oxalate while stirring, adjusting the pH value, separating liquid, washing with water, concentrating, adding
acetone, decolorizing, filtering, transferring into a reaction
bottle, heating, introducing
hydrochloric acid gas to adjust the pH value, stirring, cooling, continuing stirring for
crystallization, filtering, and
drying to obtain dioxopromethazine
hydrochloride. The whole process is free of dangerous reaction, the post-treatment method is conventional liquid separation,
salting and
crystallization, the operation is simple, and the dangerous process that oxidizing agents such as
oxygen and
hydrogen peroxide are used for oxidation reaction in the conventional synthesis process is avoided.