A kind of process method of vacuum concentration instead of rectification to produce Woshi oxide

Abstract

The invention relates to a technique for producing 16,17-epoxyprogesterone by vacuum concentration instead of flush distillation, which comprises the following steps: 1) adding 16,17-alpha-epoxyprognenolone into toluene in a reaction tank, dehydrating by heating, adding cyclohexanone, continuing heating to evaporate toluene and removal water to a clear state, adding aluminum isopropoxide when the temperature in the tank drops to lower than 95 DEG C, and heating under reflux for 2 hours to complete Oppenauer oxidation; 2) cooling the material in the step 1) to lower than 100 DEG C, adding water to destroy the aluminum isopropoxide, stirring, standing, removing the water layer, concentrating by heating in vacuum to a dry state, repeating the process of adding water and concentrating by heating in vacuum, adding ethanol, concentrating by heating in vacuum until no liquid exists, adding ethanol, heating under reflux for 60 minutes, and sucking into a refining tank; and 3) when the material in the refining tank is cooled to lower than 10 DEG C, centrifuging, filtering and drying to obtain the 16,17-epoxyprogesterone finished product. The technique provided by the invention simplifies the production process, greatly shortens the production cycle of the procedure, lowers the production cost, and improves the product quality.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and relates to a preparation method of a steroid hormone drug intermediate, in particular to a process method of producing Woshi oxide by adopting decompression concentration instead of rectification. Background technique [0002] Woshi oxide, chemical name: 16,17α-epoxy-4-pregnene-3.20-dione, Woshi oxide has the mother nucleus of cyclopentane-perhydrophenanthrene, which is a typical steroidal compound and is a synthetic Important intermediates of various corticosteroids. [0003] Woshi oxide is epoxidized by dienolone acetate (referred to as diene) with hydrogen peroxide, concentrated, Woshi oxidation reaction, sodium hydroxide destroys aluminum isopropoxide, and then distilled with water vapor, centrifuged to obtain the crude product, ethanol Refined products. It is reported in domestic and foreign literature that the post-treatment process of the Woshi oxidation reaction is to r...

AI Technical Summary

Problems solved by technology

It is reported in domestic and foreign literature that the post-treatment process of the Woshi oxidation reaction is to remove the solvent toluene by rectification. The rectification process generally takes more than 12 hours, which takes a long time, consumes a lot of energy, and is affected by the vapor pressure. Residual solvents will affect the quality of the crude product, resulting in difficulties in refining, and the increase in the amount of ethanol will directly affect the quality of the product

[0004] In summary, the existing process technology has serious shortcomings such as long cycle, high energy consumption, high production cost, complicated post-processing procedures, low yield, and unstable product quality.