This invention provides a method for preparing
androstane-3,6,17-trione (E,Z)-3-[O-(2-aminoethyl)]
oxime hydrochloride, comprising the following steps:
benzophenone oxime reacts with 2-chloroethylamine
hydrochloride in
dimethyl sulfoxide, followed by acid-base adjustment,
toluene extraction,
hydrolysis with concentrated
hydrochloric acid to remove the
protecting group, and
crystallization to obtain high-purity 2-aminoethylamine
hydrochloride;
androstane-3,6,17-
triol is used as a
raw material and oxidized under the
catalysis of
sodium bromate and
ruthenium oxide (IV), quenched, separated, washed with water, and crystallized by
solvent replacement with isopropanol to obtain
androstane-3,6,17-trione; the 2-aminoethylamine hydrochloride solution is mixed and reacted with the trione in
tetrahydrofuran solution at low temperature, followed by
salting out,
filtration, separation, washing with saturated brine and
drying with
magnesium sulfate, and purification by
solvent replacement, water
dissolution and concentration, and cooling
crystallization to obtain the high-purity target product. This invention significantly improves the yield of the target product by optimizing
reaction conditions, while achieving readily available raw materials, low cost, and industrialized production through traditional
chemical reaction pathways.