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Chemical synthesis method of methylprednisolone

A methylprednisolone, chemical synthesis technology, applied in chemical instruments and methods, organic chemistry, steroids, etc., can solve the problems of product loss, low yield, difficulty in processing and purification, etc. The effect of less product, lower production cost and higher total yield

Inactive Publication Date: 2008-07-30
TAIZHOU TAIFA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Another outstanding problem is that after the 6-position methylation reaction is completed, there are many by-products in the whole reaction system that are very close to the polarity and solubility of the final product methylprednisolone, which leads to It is very difficult to process and purify Nisolone. In order to obtain methylprednisolone with higher purity, a large amount of product is lost and the yield is relatively low.

Method used

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  • Chemical synthesis method of methylprednisolone
  • Chemical synthesis method of methylprednisolone
  • Chemical synthesis method of methylprednisolone

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Platts Oxidation

[0034] Throw in 30 kg of mold oxide, add 10 kg of glacial acetic acid, stir and cool to 0°C, add 6 kg of manganese chloride aqueous solution (containing 0.1 parts by weight of manganese chloride and 0.1 parts by weight of water in the aqueous solution of manganese chloride), and cool to 10°C 18 kg of chromic anhydride aqueous solution was added dropwise (containing 0.3 parts by weight of chromic anhydride and 0.3 parts by weight of water in the aqueous solution of chromic anhydride), the temperature was controlled at 10°C, added dropwise for 3 hours, and reacted at 25°C for 6 hours after the dropwise addition, and added 900 kg of water, stirred for 1 hour for water analysis, centrifuged after water analysis, washed the filter cake until neutral, and dried at 70°C to obtain the Platinum compound.

[0035] (2) bromine reaction

[0036] Take 27 kg of Platinum, add 100 kg by weight of hydrogen bromide, stir and heat up to 30 ° C for 4 hours, add 1000...

Embodiment 2

[0057] (1) Platts Oxidation

[0058] Throw in 30 kg of mold oxide, add 15 kg of glacial acetic acid, stir and cool to 0°C, add 6 kg of manganese chloride aqueous solution (containing 0.1 parts by weight of manganese chloride and 0.1 parts by weight of water in the aqueous solution of manganese chloride), and cool to 10°C 18 kg of chromic anhydride aqueous solution was added dropwise (containing 0.3 parts by weight of chromic anhydride and 0.3 parts by weight of water in the aqueous chromic anhydride solution), the temperature was controlled at 15°C, added dropwise for 3 hours, and reacted at 20°C for 5 hours after the dropwise addition, and added 1000 kg of water, stirred for 1 hour for water analysis, centrifuged after water analysis, washed the filter cake until neutral, and dried at 70°C to obtain the Platinum compound.

[0059] (2) bromine reaction

[0060] Take 27 kilograms of Platinum, add 135 kilograms of hydrogen bromide, stir and heat up to 35 ° C for 4 hours, add 13...

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Abstract

The invention discloses a chemical synthesis method of methylpredmisolone. Fungi oxide is adopted as the initial material and methylpredmisolone is obtained after prevotella oxidation, bromine application, bromine removal, 6-bit methylenation, 6-bit methylation, ketal protection, 11- bit reduction, ketal hydrolization, 1 and 2 bit dehydrogenation, 21-bit iodine application, 21-bit permutation and 21-bit hydrolytic reaction. The flow of the synthesis method of the invention is reasonable, the yield rate and the purity of the intermediate products are high, the reaction condition is temperate, the by-products in the end product are few, the purity is high (reaching above 98 percent), the industrialization is easy to be realized, thereby the method has high application value.

Description

technical field [0001] The invention relates to a method for synthesizing methylprednisolone (1,4-pregnadiene-3,20-dione-11β,17α,21-triol-6α-methyl). Background technique [0002] Methylprednisolone is the key intermediate for the production of the highly efficient glucocorticoid methylprednisolone sodium succinate. It has anti-inflammatory, anti-cellular immune effects and good curative effect. It is the first choice commonly used in the treatment of nephrotic syndrome medicine. [0003] The production of methylprednisolone has been monopolized by the U.S. Upjohn Company for many years, and downstream products and preparations also mainly rely on imports. [0004] Disclosed a kind of chemical synthesis method of methylprednisolone in Chinese invention patent application (publication number CN1763066), take pregnane dienolone acetate as starting raw material, through epoxidation, Wo Shi reaction, mold oxidation, Platts reaction, upper debromination, upper iodine replacemen...

Claims

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Application Information

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IPC IPC(8): C07J71/00C07J75/00
Inventor 汪家振
Owner TAIZHOU TAIFA PHARMA
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