The invention relates to the technical field of
vitamin intermediates, and particularly discloses a preparation process of a
vitamin D3 key intermediate 7-p-toluenesulfonyl epide-3-
cholesteryl ester. The invention relates to a preparation process of a
vitamin D3 key intermediate 7-p-toluenesulfonylepide-3-
cholesteryl ester, which comprises the following steps: reaction: adding 7-keto-3-
cholesteryl ester, p-toluenesulfonhydrazide and concentrated
hydrochloric acid into
methanol, heating to 45-50 DEG C, and carrying out heat preservation reaction for 6.5-7.5 hours; post-treatment: after the reaction is finished, cooling
crystallization and suction
filtration are performed to obtain a
solid, the
solid is eluted by using iced
methanol, suction
drying is performed to obtain a washing solution and a
filter cake, and the
filter cake is subjected to
vacuum drying to constant weight to obtain the product 7-p-toluenesulfonylepide-3-cholesteryl ester. The concentrated
hydrochloric acid is used as a catalyst, and the reaction is carried out at 45-50 DEG C for 6.5-7.5 h, so that the reaction is mild, the
energy consumption is reduced, and the production efficiency of the 7-p-toluenesulfonylepide-3-cholesteryl ester is improved.