Preparation technique for high-purity hydrocortisone

A technology of hydrocortisone and preparation process, which is applied in the directions of organic chemistry, steroids, etc., can solve the problems of high toxicity to operators, inconvenient procurement and transportation, and inability of medicines to pass through, so as to achieve low comprehensive cost and low toxicity. , safe to use

Active Publication Date: 2009-12-16
云南泽维制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the hydrocortisone that dichloroethane is made as separation solvent has following problems: 1, dichloroethane as solvent is a kind of poisonous solvent of bad-smelling gas, belongs to a class of solvents, relatively harmful to the health of operators 2. It is prohibited to use in the production of raw materials, and cannot pass the drug registration certification
3. There are many impurities greater than 0.1%, which brings great difficulties to FDA or COS registration certification
4. The operation is difficult, dichloroethane and methanol are incompatible with each other, and the error is large when the specific gravity is detected by the central control, which has a great impact on production
5. Dichloroethane is highly toxic, and it is inconvenient to purchase and transport

Method used

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  • Preparation technique for high-purity hydrocortisone
  • Preparation technique for high-purity hydrocortisone
  • Preparation technique for high-purity hydrocortisone

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Put 30g of crude hydrocortisone, 358g of dichloromethane, and 95g of methanol into the reaction tank for one separation, stir, heat at 32°C and reflux for 20min, cool down to 0°C and keep for 20min, add 105g of water to dilute, continue to cool down for 1 hour, let stand for 1 hour, and centrifuge Dry put into secondary separation, add 135g of dichloromethane, 36g of methanol, stir, heat at 32°C and reflux for 20min, cool down to 0°C and keep for 20min, add 54g of water to dilute, continue to cool down for 1 hour, let stand for 1 hour, and centrifuge and dry to obtain hydrocortisone isolate 12.7g. The quality is acceptable.

Embodiment 2

[0026] Put 30g of crude hydrocortisone, 199g of dichloromethane, and 50.4g of methanol into the reaction tank for one separation, stir, heat at 32°C and reflux for 20min, cool down to 0°C and keep for 20min, add 105g of water to dilute, continue to cool down for 1 hour, let stand for 1 hour, and centrifuge Spin dry and put into secondary separation, add 120.6g of dichloromethane, 28.8g of methanol, stir, heat at 32°C and reflux for 20min, cool down to 0°C and keep for 20min, add 55g of water to dilute, continue to cool down for 1 hour, let it stand for 1 hour, and centrifuge and dry to obtain hydrogenated cocoa The loose isolate was 17.5g, and the quality was qualified.

Embodiment 3

[0028] Put 30g of crude hydrocortisone, 240g of dichloromethane, and 60g of methanol into the reaction tank for one separation, stir, heat at 32°C and reflux for 20min, cool down to 0°C and keep for 20min, add 105g of water to dilute, continue to cool down for 1 hour, let stand for 1 hour, and centrifuge Dry put into secondary separation, add 126g of dichloromethane, 32.4g of methanol, stir, heat at 32°C and reflux for 20min, cool to 0°C and keep for 20min, add 60g of water to dilute, continue to cool down for 1 hour, stand still for 1 hour, and centrifuge and dry to obtain hydrocortisone separation The product is 16.9g, and the quality is qualified.

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Abstract

The invention discloses a process for the separation and preparation of refined high-purity hydrocortisone, using low-toxic solvent dichloromethane instead of dichloroethane, one separation process in the process: the weight ratio of raw materials is crude hydrocortisone: dichloromethane Methane:methanol:water=1:6.6-11.9:1.68-3.16:3-3.5. Secondary separation process: the weight ratio of raw materials is hydrocortisone primary isolate: dichloromethane: methanol: water=1: 6.7~7.5: 1.6~2: 3~3.5; hydrocortisone crude product, dichloromethane Add methane, methanol, and water into the reaction tank according to the weight ratio, raise the temperature and reflux, lower the temperature, add a certain amount of water to dilute, and let it stand still. After two separation processes, the high-purity hydrocortisone is obtained after refining.

Description

technical field [0001] The invention belongs to the technical field of chemical medicine production technology, and relates to a production and preparation process of high-purity hydrocortisone. Background technique [0002] Drug Hydrocortisone Hydrocortisone, the chemical name is 11β, 17α, 21-trihydroxypregna-4-ene-3,20-dione. Also known as: Cortisone; Cortisol; Hydrocortisol; Hydrocortisone, etc. Its structural formula: [0003] [0004] Molecular formula: C21H30O5. Relative molecular weight: 362.47. As an important variety of steroidal corticosteroids, hydrocortisone is widely used in the treatment of adrenal insufficiency and autoimmune diseases, and it is also an intermediate for further synthesis of other drugs. Therefore, my country, the United States, the Netherlands, Germany, Russia, Poland, and other countries have always attached great importance to the research on the production technology of hydrocortisone. The United States is the largest producer of st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J5/00
Inventor 谭志云李奇
Owner 云南泽维制药有限公司
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