Preparation method and application of catalyst for hydrogenation of steroid compounds

Abstract

The invention discloses a preparation method of a catalyst for hydrogenation of steroid compounds. The method comprises the following steps: 1, pretreating active carbon; 2, dissolving a dissoluble palladium compound and dissoluble salt of an auxiliary agent into water and stirring uniformly to obtain a precursor solution; 3, adding a pretreated active carbon carrier into the precursor solution, dipping, adjusting the pH value of a dipping system, continuously stirring for 1 to 5 hours, filtering and washing a filter cake; and 4, pulping the filter cake which is washed to be neutral with pure water to obtain pulp, adjusting the pH value of the pulp, adding a reducing agent to reduce the pulp, filtering, washing and drying to obtain the catalyst for hydrogenation of the steroid compounds. In addition, the invention also discloses a method for catalyzing hydrogenation of the steroid compounds by using the catalyst. The catalyst prepared by the method is applicable to catalytic hydrogenation of the steroid compounds; the yield of products exceeds 95 percent; the mass percentage content of isomers in the products is less than 5 percent; and the catalyst has stable performance and good repeatability.

Description

technical field [0001] The invention belongs to the technical field of preparation of noble metal catalysts, and in particular relates to a preparation method and application of a catalyst for hydrogenation of steroid compounds. Background technique [0002] Steroids are the second largest class of drugs after antibiotics. After decades of research and development, steroidal drugs have formed a large class of drugs with a wide variety of clinical applications, mainly for the treatment of rheumatism, cardiovascular, collagenous diseases, lymphatic leukemia, tumors, bacterial encephalitis , skin diseases, endocrine disorders, senile diseases, etc. From the perspective of the development of the international steroid drug industry, sales in 2006 have reached 40 billion US dollars, accounting for about 10% of the world's sales of pharmaceutical products. my country's annual output value exceeds 18 billion yuan, accounting for 7% of the total output value of the pharmaceutical i...

AI Technical Summary

Problems solved by technology

However, the preparation process of this catalyst is complicated, and nitrogen protection is required in this process, which has certain limitations on the large-scale industrialization of this catalyst.

[0005] Chinese patent CN102603841A has reported another preparation method for the preparation of steroid drug intermediates, wherein NaBH 4 or KBH 4 It is a reducing agent, but there are many experimental steps and complicated process, the yield of the final target product is only about 80%, and the catalyst can only be used once, which is easy to decompose

[0006] In addition, Chinese patents such as CN101177443A, CN101362789A, CN102212099A and CN101717422A have all studied the preparation process of steroidal drugs respectively, but these preparation methods all have the same reaction disadvantage: each complementary reaction product is sensitive to temperature and is not easy to control, and the product yield is only about 70%

[0007] Document DE3427468, patent US2857337 and patent US3138560 have studied the preparation process and technology of the catalyst used in the preparation process of steroid drug intermediates, but the activity and stability of the catalyst prepared by this method are relatively poor, and the target Product selectivity is poor

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