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Methylprednisolone production method and production device

A technology for methylprednisolone and production equipment, which is applied in the directions of drying gas arrangement, steroid, non-progressive dryer, etc., can solve the damage to the shape and structure variation of intermediate products, reduce the production quality of methylprednisolone, and reduce methylprednisolone. Crystallization instability and other problems, to avoid morphological changes, speed up drying, shorten production time

Active Publication Date: 2018-11-30
YUEYANG HUANYU PHARMA +6
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the production of traditional methylprednisolone, due to the need to adopt multi-step chemical reactions for production, the intermediate product raw materials formed need to be dried multiple times, while the existing drying equipment generally adopts electric resistance wire heating and drying or complete vacuum pumping. Pressure dehumidification, heating and drying of electric heating resistance wire are likely to have a relatively large negative impact on the intermediate product of methylprednisolone preparation, which makes the structure of the intermediate product change, and eventually leads to the instability of subsequent methylprednisolone crystallization and the decrease in purity. Electric resistance wire heating drying equipment or vacuum negative pressure dehumidification equipment have a long drying time. Although vacuum pumping negative pressure dehumidification can achieve rapid dehumidification by rapid decompression, rapid decompression is easy to change the shape and structure of intermediate products. Mutation damage occurs, which reduces the quality of subsequent methylprednisolone production

Method used

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  • Methylprednisolone production method and production device
  • Methylprednisolone production method and production device
  • Methylprednisolone production method and production device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075]The process embodiment one of producing methylprednisolone, it comprises following preparation steps:

[0076] Ketal reaction: 160 parts of ethylene glycol, 160 parts of triethyl orthoformate, 130 parts of Platts debrominated product, 2 parts of trimethyl sulfoxide bromide were pumped into the reactor, reacted for 5 hours, and triethylamine was added , neutralized to neutral, crystallized, centrifugally dried, put into the drying equipment, start the infrared heating tube 6, irradiate for 5 minutes, control the speed of the motor 19 to 900-1000r / min, and continue to run for 10 minutes to obtain shrinkage Ketones;

[0077] The reaction formula is:

[0078]

[0079] Reduction reaction: pump 800 parts of tetrahydrofuran into the reaction kettle, add 450 parts of the ketal product, 15 parts of sodium borohydride, react for 12 hours, add 6 parts of glacial acetic acid, concentrate and dry tetrahydrofuran under negative pressure, add water for water analysis, centrifuge, ...

Embodiment 2

[0100] The process embodiment two of producing methylprednisolone, it comprises following preparation steps:

[0101] Ketal reaction: pump 200 parts of ethylene glycol, 200 parts of triethyl orthoformate, 170 parts of Platts debrominated product, 4 parts of trimethylsulfoxide bromide into the reactor, react for 7 hours, add triethylamine , neutralized to neutral, crystallized, centrifugally dried, put into the drying equipment, start the infrared heating tube 6, irradiate for 5 minutes, control the speed of the motor 19 to 900-1000r / min, and continue to run for 10 minutes to obtain shrinkage Ketones;

[0102] Reduction reaction: pump 1000 parts of tetrahydrofuran into the reaction kettle, add 550 parts of the ketal product, 20 parts of sodium borohydride, react for 12 to 15 hours, add 10 parts of glacial acetic acid, concentrate and dry tetrahydrofuran under negative pressure, add water for water analysis, After centrifugation and drying, put it into the drying equipment, sta...

Embodiment 3

[0109] The process embodiment three of producing methylprednisolone, it comprises following preparation steps:

[0110] Ketal reaction: pump 180 parts of ethylene glycol, 180 parts of triethyl orthoformate into the reactor, add 150 parts of Platts debrominated product, 3 parts of trimethylsulfoxide bromide, control the temperature at 32-35 °C, and react After 6 hours, add triethylamine, neutralize until the pH is 8, drop to 5-10°C, crystallize for 1 hour, spin dry by centrifugation, put it into the drying equipment, start the infrared heating tube 6, irradiate for 5 minutes, control The rotating speed of the motor 19 is 900-1000r / min, and it runs continuously for 10 minutes to obtain the ketal product;

[0111] Reduction reaction: pump 900 parts of tetrahydrofuran into the reaction kettle, add 516 parts of the ketal product, 18 parts of sodium borohydride, heat up to 65-68°C for reflux reaction for 12-15 hours, point the board to confirm that the raw materials have been reacte...

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Abstract

The invention discloses a methylprednisolone production device, which comprises a reaction kettle, an elutriation kettle, a centrifugal filtration device, a concentration kettle, a decoloration kettle, a biological fermentation tank and a drying device which are connected in sequence, wherein the drying device comprises an outer cylinder, a drying cylinder and an inner cylinder; a motor is arranged on the bottom surface of the outer cylinder; an exhaust fan blade, a cylinder type impeller and a vortex impeller are arranged on a motor rotating shaft; the exhaust fan blade is arranged between the drying cylinder and the bottom surface of the outer cylinder; the cylinder type impeller is arranged between the drying cylinder and the inner cylinder; the vortex impeller is arranged at the bottomof the inner cylinder; an infrared heating pipe is arranged on the top surface of the inner cylinder; a feeding port is formed in the center of the upper end of the inner cylinder; the side wall of the outer cylinder comprises an inner layer wall and an outer layer wall; an annular interlayer cavity is formed between the inner layer wall and the outer layer wall; an annular baffle is arranged atthe outlet of the upper end of the interlayer cavity, a vent is formed in the baffle, and a rotatable air purification ring is arranged at the upper end of the baffle. According to the method, the preparation time of intermediate products in the production process of the methylprednisolone can be reduced, and rapid and high-quality production of the methylprednisolone can be realized.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical production, in particular to a methylprednisolone production process and a production device. Background technique [0002] Methylprednisolone is a medium-efficiency synthetic product, which belongs to the adrenal cortex hormone drugs in the endocrine system drugs. The anti-inflammatory effect of 4mg is about the same as that of 5mg prednisolone. The sodium retention effect is weak, and it is white or almost white crystalline Powder, odorless, initially tasteless and then bitter. Soluble in absolute ethanol and chloroform, almost insoluble in water, used for first aid for critical illnesses, 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 u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00F26B11/10F26B21/00F26B25/04
CPCC07J5/0053F26B11/10F26B21/001F26B25/04
Inventor 韩朝东辛俊浩别春梅秦郁薛晓霞杨月霞徐润星
Owner YUEYANG HUANYU PHARMA
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