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Refining method of difluprednate

A technology of difluprednate and refining method, applied in the directions of steroids, organic chemistry, etc., can solve problems such as increasing processing cost, and achieve the effects of improving product quality, reducing the number of refining times, and simple operation

Active Publication Date: 2022-07-05
HENAN LIHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In many refining methods, in order to ensure that the impurities meet the requirements, the yield is often sacrificed, and the yield is usually only about 80%, which greatly increases the processing cost

Method used

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  • Refining method of difluprednate
  • Refining method of difluprednate
  • Refining method of difluprednate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Add 20 g of the dry crude product of difluprednate and 100 mL of dichloromethane into a dry and clean reaction flask, stir and heat up to 30°C to completely dissolve the dry product of crude difluprednate; after dissolving, add 1 g to the system activated carbon, and refluxed at 37 °C for 1 h for decolorization, and then at 35 °C for insulation filtration to obtain the decolorized difluprednate dichloromethane solution; decolorize the decolorized difluprednate dichloromethane solution. Pressure distillation, control the distillation temperature to be about 25 ° C, the vacuum degree is -0.07 MPa, and vacuum distillation to a solution volume of about 30 mL, then add 80 mL of methanol to the concentrated difluprednate dichloromethane solution, and control the distillation temperature. About 50 ℃, the vacuum degree is -0.07MPa, when the solution volume is about 50mL by vacuum distillation, then 120mL petroleum ether is added to the concentrated difluprednate dichloromethane ...

Embodiment 2

[0056] Add 20 g of the dry crude product of difluprednate and 100 mL of dichloromethane into a dry and clean reaction flask, stir and heat up to 30 °C to completely dissolve the dry product of crude difluprednate; after dissolving, add 2 g of 2 g to the system activated carbon, and refluxed at 35 °C for 1 h for decolorization, and then at 35 °C for insulation filtration to obtain a decolorized difluprednate dichloromethane solution; decolorize the decolorized difluprednate dichloromethane solution. Pressure distillation, control the distillation temperature to be about 30 ° C, the vacuum degree is -0.08 MPa, and vacuum distillation to a solution volume of about 30 mL, then add 100 mL of methanol to the concentrated difluprednate dichloromethane solution, and control the distillation temperature. About 45 ℃, the vacuum degree is -0.08MPa, when the solution volume is about 60mL by vacuum distillation, then 130mL petroleum ether is added to the concentrated difluprednate dichlorom...

Embodiment 3

[0059] Add 20 g of the dry crude product of difluprednate and 120 mL of dichloromethane into a dry and clean reaction flask, stir and heat up to 25°C to completely dissolve the crude product of difluprednate; after dissolving, add 1 g of activated carbon, and refluxed at 40 °C for 0.5 h for decolorization, and then filtered at 40 °C to obtain the decolorized difluprednate dichloromethane solution; the decolorized difluprednate dichloromethane solution was subjected to Under reduced pressure distillation, control the distillation temperature to be about 35 ° C, the vacuum degree is -0.06MPa, when the vacuum distillation is carried out to the solution volume of about 35 mL, then add 90 mL of methanol to the concentrated difluprednate dichloromethane solution, and control the distillation The temperature is about 50°C, the degree of vacuum is -0.06MPa, and the solution is distilled under reduced pressure to a volume of about 50mL, then 130mL of petroleum ether is added to the conc...

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Abstract

The invention provides a refining method of difluprednate. The refining method of the difluprednate comprises the following steps: S1, adding dichloromethane into a difluprednate crude product, decolorizing, filtering and concentrating to obtain a concentrated difluprednate dichloromethane solution; s2, methanol is added into the concentrated difluprednate dichloromethane solution, and a concentrated difluprednate dichloromethane and methanol mixed solution is obtained through concentration; and S3, adding petroleum ether into the concentrated difluprednate dichloromethane and methanol mixed solution, concentrating, stirring for crystallization, standing, filtering and drying to obtain a refined difluprednate product. According to the refining method, the yield of the difluprednate is 95% or above, the content of the difluprednate is 99.7% or above, the impurity content is smaller than 0.1%, the high yield is guaranteed while the quality of the difluprednate product is improved, and the refining cost is reduced.

Description

technical field [0001] The invention relates to the technical field of drug purification, in particular to a purification method of difluprednate. Background technique [0002] Steroid drugs are the second largest class of drugs in the world after antibiotics in sales, and their molecular structures can be derived from steroid hormone intermediates. Difluprednate is a steroid drug with the following structural formula: [0003] [0004] Difluprednate is a topical steroidal anti-inflammatory drug designed and developed under the "soft drug" concept. Compared with other ophthalmic steroid drugs, it has high lipophilicity and easy decomposition, and long-term use will not cause increased intraocular pressure in patients, so the side effects are lower. From a structural point of view, difluprednate is a difluoro derivative of hydrocortisone, which has anti-inflammatory activity, especially the fluorination treatment at the C9 position, which can significantly enhance the an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
CPCC07J5/0053
Inventor 李世玉陈文霞潘严彬
Owner HENAN LIHUA PHARMA
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