Method for preparing 6 beta-methylprednisolone

A technology of methylprednisolone and methyl, which is applied in the field of chemical preparation, can solve the problem of the difficulty in ensuring the purity and pharmacological activity of methylprednisolone, and the inability to prepare 6β-methylprednisolone reference substances, etc. problem, to achieve the effect of improving purity and pharmacological activity

Inactive Publication Date: 2018-01-19
ZHEJIANG XIANJU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the technical problem that the 6β-methylprednisolone reference subs...

Method used

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  • Method for preparing 6 beta-methylprednisolone
  • Method for preparing 6 beta-methylprednisolone

Examples

Experimental program
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Embodiment 1

[0036] The first step, Grignard, hydrolysis, and elimination: In a 250mL dry reaction bottle, add tetrahydrofuran (53mL, 5.3V), then add magnesium flakes (6.7g, 0.67W), pass through monochloromethane until the temperature rises rapidly to 55-61 °C, lower the temperature until the reaction is stable. Add tetrahydrofuran (80mL, 8V) into the reaction flask, keep warm at 30-50°C and ventilate until the magnesium dissolves, then ventilate for 6-8 hours, then inject about 20g of monochloromethane (20g, 2W), and store in airtight. Then concentrate under normal pressure and distill off tetrahydrofuran until the temperature rises to 71-74°C. After cooling down to room temperature, it was protected with nitrogen gas and sealed for use. Add tetrahydrofuran (20mL, 2V) into a 250mL reaction flask, add 6-methylepoxide 1 (10g, 1W), stir for 20-30 minutes, then slowly add Grignard reagent (60mL, 6V), heat and reflux for 4 ~5 hours, cool to below 20°C; add glacial acetic acid (20mL, 2V), ice...

Embodiment 2

[0050] The first step, Grignard, hydrolysis, and elimination: In a 250mL dry reaction bottle, add tetrahydrofuran (53mL, 5.3V), then add magnesium flakes (6.7g, 0.67W), pass through monochloromethane until the temperature rises rapidly to 55-61 °C, lower the temperature until the reaction is stable. Add tetrahydrofuran (80mL, 8V) into the reaction flask, keep warm at 30-50°C and ventilate until the magnesium dissolves, then ventilate for 6-8 hours, then inject about 20g of monochloromethane (20g, 2W), and store in airtight. Then concentrate under normal pressure and distill off tetrahydrofuran until the temperature rises to 71-74°C. After cooling down to room temperature, it was protected with nitrogen gas and sealed for use. Add tetrahydrofuran (20mL, 2V) into a 250mL reaction flask, add 6-methylepoxide 1 (10g, 1W), stir for 20-30 minutes, then slowly add Grignard reagent (60mL, 6V), heat and reflux for 4 ~5 hours, cool to below 20°C; add glacial acetic acid (20mL, 2V), ice...

Embodiment 3

[0053] The first step, Grignard, hydrolysis, and elimination: In a 250mL dry reaction bottle, add tetrahydrofuran (53mL, 5.3V), then add magnesium flakes (6.7g, 0.67W), pass through monochloromethane until the temperature rises rapidly to 55-61 °C, lower the temperature until the reaction is stable. Add tetrahydrofuran (80mL, 8V) into the reaction flask, keep warm at 30-50°C and ventilate until the magnesium dissolves, then ventilate for 6-8 hours, then inject about 20g of monochloromethane (20g, 2W), and store in airtight. Then concentrate under normal pressure and distill off tetrahydrofuran until the temperature rises to 71-74°C. After cooling down to room temperature, it was protected with nitrogen gas and sealed for use. Add tetrahydrofuran (20mL, 2V) into a 250mL reaction flask, add 6-methylepoxide 1 (10g, 1W), stir for 20-30 minutes, then slowly add Grignard reagent (60mL, 6V), heat and reflux for 4 ~5 hours, cool to below 20°C; add glacial acetic acid (20mL, 2V), ice...

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Abstract

The invention discloses a method for preparing 6 beta-methylprednisolone. The method comprises the following steps: taking 6-methyl epoxides as raw materials, after Grignard reaction, hydrolysis, elimination, generating 6 beta-methyl elimination, and then after dehydrogenation by fermentation, iodine putting, replacement, hydrolysis, preparation of liquid phase purification, obtaining 6 beta-methylprednisolone. A reaction formula is as follows: the formula is shown in the description, the 6 beta-methylprednisolone of the invention is a major synthetic impurity in methylprednisolone, separation and purification of the 6 beta-methylprednisolone have great significance on impurity analysis.

Description

technical field [0001] The invention relates to a method for preparing chemicals, in particular to a method for preparing 6β-methylprednisolone. Background technique [0002] Methylprednisolone belongs to the class of glucocorticoids and is used for emergency treatment of critical illnesses. It can also be used for endocrine disorders, rheumatic diseases, collagen venereal diseases, skin diseases, allergic reactions, eye diseases, gastrointestinal diseases, blood diseases, Leukemia, shock, cerebral edema, polyneuritis, myelitis, and prevention of vomiting caused by cancer chemotherapy. At present, it is mainly used clinically for organ transplantation. 6β-Methylprednisolone is an important impurity in the finished product of methylprednisolone and has no pharmacological activity. In order to better control the quality of methylprednisolone, the impurities therein must be controlled, so it is necessary to prepare this substance as a reference substance. [0003] Due to the...

Claims

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Application Information

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IPC IPC(8): C07J5/00
Inventor 刘东华戴静方伟明
Owner ZHEJIANG XIANJU PHARMA
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