The invention discloses a preparation method of a
vitamin B2 diastereoisomer, which comprises the following steps: adding absolute ethyl
alcohol into a high-pressure reaction kettle, adding 3, 4-
dimethylaniline, D-
arabinose and
palladium carbon in a stirring state, introducing
hydrogen, heating for reaction, and filtering while hot; cooling, crystallizing and filtering the filtrate, collecting a
filter cake, dissolving the
filter cake with a
hydrochloric acid aqueous solution, adding
aniline diazonium salt in a stirring state, after the reaction is completed, adding
sodium acetate for crystallizing and filtering, and adding the
filter cake into a
mixed solution of a
solvent A and
barbituric acid for
reflux reaction; cooling to
room temperature and filtering to obtain a
vitamin B2 diastereoisomer crude product; adding inorganic acid B into the crude wet filter cake for dissolving, adding into hot water, filtering while hot, and
drying the diastereoisomer of the
vitamin B2. The whole process steps are simple and easy to operate, all the raw materials required for preparation are common and easily available
raw material substances, and meanwhile, the
vitamin B2 diastereoisomer prepared by the whole preparation process is relatively high in purity, so that the whole preparation efficiency and quality are ensured.