Method for preparing cortisone acetate in one pot

Abstract

Provided is a method for preparing cortisone acetate in one pot. According to the method, Anecortave acetate is adopted as a raw material, and after the raw material is added into an organic solvent,a pot is adopted for preparation. The method comprises the following steps of A, adding a compound I into a mixed organic solvent and adding a halogenating reagent and an acid catalyst, wherein the reaction temperature is controlled in a range from -10 DEG C to 30 DEG C; after the reaction is finished, adding a quencher to quench the reaction, wherein the quencher comprises a sodium sulfite solution or a sodium bisulfite solution; B, adding an oxidant into a system finally obtained in step A, wherein the oxidant is a Jones reagent or pyridine chlorochromate or a Dess-Martin oxidant used for anoxidization reaction, and the reaction temperature is controlled in a range from -10 DEG C to 30 DEG C; after the reaction is finished, adding the quencher to quench the reaction; C, adding an organic acid catalyst and a reducing agent into an organic layer finally obtained in step B to obtain a target product cortisone acetate IV. The preparation method greatly reduces the discharge amount of waste liquid.

Description

technical field [0001] The invention relates to drug synthesis, in particular to a method for preparing cortisone acetate, which belongs to the field of chemical technology. Background technique [0002] Cortisone Acetate (Cortisone Acetate), also known as corticosterone acetate (Adreson), is a steroid hormone It is an important intermediate in the class of APIs, and can be used to synthesize various high value-added APIs such as prednisone acetate and hydrocortisone. At present, it is recorded in Chinese, American and European pharmacopoeias. Cortisone acetate is a medium-acting adrenal cortex hormone drug, which acts on glucose metabolism and has a certain impact on electrolyte metabolism. For severe bronchial asthma, severe dermatitis and other allergic diseases, active rheumatism, rheumatoid arthritis, lupus erythematosus and other diseases. [0003] Chinese patents CN201210496816.9 and CN201410150052.7 relate to the synthesis of cortisone acetate intermediates and cor...

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Problems solved by technology

[0003] Chinese patents CN201210496816.9 and CN201410150052.7 relate to the synthesis of cortisone acetate intermediates and cortisone acetate, which use 4-pregnene-11α, 17α-dihydroxy-3,20-dione as raw materials. Cortisone acetate is prepared by oxidation, iodine addition, replacement and other reactions. Although the synthesis steps of the above route are short, the starting material needs to undergo biological fermentation, and the fermentation process is more complicated. At the same time, the reaction still uses iodine, which still has high cost and waste water volume. big problem

[0007] The process introduced by this method has been greatly improved on the previous basis, but there are still many problems, including complicated post-treatment, organic solvents are not recycled, etc., each step still produces a large amount of waste water, which is more harmful to the environment. Serious; and each step needs to be centrifugally discharged, which will cause the loss of the target product, waste manpower, material resources and energy, which does not conform to the concept of energy saving, environmental protection and green development

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