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Preparation method of important intermediate of cortisone acetate

A technology of cortisone acetate and intermediates, which is applied in the field of preparation of cortisone acetate intermediates, can solve the problems of increasing the difficulty of wastewater treatment and the high price of TEMPO, and achieve good industrial application prospects and value, cost, and low price Effect

Active Publication Date: 2015-04-01
JIANGSU YUANDA XIANLE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

TEMPO in this method is expensive, and chloroform is a class of solvent known to be carcinogenic and strongly suspected to be harmful to humans and the environment. It is easily decomposed into phosgene, which limits its production and application in the modern industry that promotes green environmental protection.
In addition, the wastewater of this process contains more inorganic salts containing halogen, which greatly increases the difficulty of wastewater treatment.

Method used

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  • Preparation method of important intermediate of cortisone acetate
  • Preparation method of important intermediate of cortisone acetate
  • Preparation method of important intermediate of cortisone acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] A kind of preparation method of cortisone acetate intermediate, operates according to the following steps:

[0052] (1) Preparation of oxidizing reagent A

[0053] In the preparation tank, add 50Kg of water, then slowly add 3.6 Kg of concentrated hydrochloric acid, and stir for ten minutes. Then add 5Kg of potassium dichromate and stir to dissolve. Cool down to 10~15°C to obtain oxidizing reagent A—potassium dichromate solution. spare.

[0054] (2) Preparation of oxide 17α-hydroxypregn-4-ene-3,11,20-trione

[0055] In the reaction tank, add 200Kg tetrahydrofuran, 20Kg glacial acetic acid, 1Kg manganese chloride and 10 Kg raw material 11α, 17α-dihydroxypregna-4-ene-3,20-dione, stir to dissolve, and control the temperature at 0~ 5°C. Add the prepared potassium dichromate solution dropwise, control the temperature below 25°C, and complete the dropwise addition in about 2 hours. Stirring, thin-layer chromatography analysis, until the reaction of raw materials is compl...

Embodiment 2

[0057] A kind of preparation method of cortisone acetate intermediate, operates according to the following steps:

[0058] (1) Preparation of oxidizing reagent A

[0059] In the preparation tank, add 20Kg of water, then slowly add 5 Kg of concentrated nitric acid, and stir for ten minutes. Then add 4.8Kg manganese oxide, stir to dissolve. Cool down to 10~15°C to obtain oxidizing reagent A—manganese oxide solution. spare

[0060] (2) Preparation of oxide 17α-hydroxypregn-4-ene-3,11,20-trione

[0061] In the reaction tank, add 250Kg acetone, 10Kg glacial acetic acid, 1.2Kg manganese chloride and 10 Kg raw material 11α, 17α-dihydroxypregna-4-ene-3,20-dione, stir to dissolve, and control the temperature at 0 ~5°C. Add the prepared manganese oxide solution dropwise, control the temperature below 25°C, and complete the dropwise addition in about 1.5 hours. Stirring, thin-layer chromatography analysis, until the reaction of raw materials is complete. 5Kg aqueous solution of so...

Embodiment 3

[0063] A kind of preparation method of cortisone acetate intermediate, operates according to the following steps:

[0064] (1) Preparation of oxidizing reagent A

[0065] In the preparation tank, add 5Kg of water, then slowly add 5 Kg of concentrated sulfuric acid, and stir for ten minutes. Add 6Kg of chromium trioxide again, stir and dissolve. Cool down to 10~15°C to obtain oxidizing reagent A—chromium trioxide solution. spare

[0066] (2) Preparation of oxide 17α-hydroxypregn-4-ene-3,11,20-trione

[0067] In the reaction tank, add 250Kg dioxane, 5Kg glacial acetic acid, 1.5Kg manganese chloride and 10 Kg raw material 11α, 17α-dihydroxypregna-4-ene-3,20-dione, stir to dissolve, control The temperature is 10~15°C. Add the prepared chromium trioxide solution dropwise, control the temperature below 15°C, and complete the dropwise addition in about 0.5 hours. Stirring, thin-layer chromatography analysis, until the reaction of raw materials is complete. Add an aqueous solut...

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Abstract

The invention relates to a preparation method of an important intermediate of cortisone acetate, and in particular relates to a preparation method of cortisone acetate intermediate 17alpha-hydroxypregnen-4-alkene-3,11,20-triketone. The preparation method comprises the following steps of (1) preparing an oxidization reagent A; (2) oxidizing 11alpha, 17 alpha-dihydroxypregnen-4-alkene-3,20-diketone to generate 17alpha-hydroxypregnen-4-alkene-3,11,20-triketone. According to the invention, the problem that industrialized production of 17alpha-hydroxypregnen-4-alkene-3,11,20-triketone in a proper workshop is carried out is solved, so the preparation method disclosed by the invention has the characteristics of lower cost and proper yield, and is more suitable for industrialized large-scale production; the reference quality yield of the 17alpha-hydroxypregnen-4-alkene-3,11,20-triketone obtained by the preparation method is 90-100%, and the reference high performance liquid chromatography purity of the 17alpha-hydroxypregnen-4-alkene-3,11,20-triketone is 95-99.9%.

Description

technical field [0001] The invention relates to the field of preparation of a cortisone acetate intermediate, in particular to a preparation method of a cortisone acetate intermediate-17α-hydroxypregna-4-ene-3,11,20-trione. Background technique [0002] Steroid hormones have strong anti-infection, anti-allergic, anti-viral and anti-shock pharmacological effects, and are important drugs for treating rheumatism, cardiovascular, lymphoid leukemia, cellular encephalitis, skin diseases, anti-tumor and rescuing critically ill patients. Among them, cortisone acetate, an important steroid drug, is mainly used for the treatment of primary or secondary adrenal insufficiency, and various types of congenital adrenal hyperplasia caused by defects in the enzyme system required for the synthesis of glucocorticoids. Its pharmacological effects can also be used to treat various diseases when necessary. The chemical structural formula of cortisone acetate is: [0003] . [0004] An impor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J7/00
Inventor 冯永华廖高荣姚庆旦
Owner JIANGSU YUANDA XIANLE PHARMA
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