The invention discloses a preparation method of DHEA (
dehydroepiandrosterone) intermediate 3 beta-acetoxyl-
androstane-3,5-
diene-17-
ketone. The preparation method is characterized in that
esterification reaction reagent is
isopropenyl acetate. The preparation method comprise the following steps of dissolving 1W of 4AD (4-androstenediol) into 3-8V of
organic solvent, wherein W is weight g, and V is volume ml; adding 1-5w% strong acidic catalyst, stirring and heating up to the
reaction temperature of 40-80 DEG C; dripping 0.5-1.2 V of
isopropenyl acetate, preserving heat and reacting for 1-2 hours after dripping, until displaying completion of reaction of raw materials by TLC (
Thin Layer Chromatography); adding 2-6% V
triethylamine for
neutralization after reaction, and concentrating the
solvent to dry; adding 1V of methyl
alcohol, dissolving while stirring, cooling to crystallize for 2-3 hours, filtering, performing
solvent washing, and baking to dry below 70 DEG C, thereby obtaining the DHEA intermediate 3 beta- acetoxyl-
androstane-3, 5-
diene-17-
ketone. The DHEA intermediate prepared by the invention has high yield, high purity and steady
mass, and can be baked under normal pressure; more importantly,
solvent recovery rate is high, and the preparation method almost produces no
wastewater, is economic and environmental friendly, and is very beneficial to industrial production.