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Chemical Synthesis Process of Prednisolone Acetate Valerate

A kind of technology of prednisolone acetate valerate and prednisolone valerate is applied in the chemical synthesis process field of prednisolone acetate valerate, which can solve the problem of high cost, difficulty in mastering the technical process, and unsuitable Large-scale production and other issues, to achieve the effects of high yield and product purity, good market application prospects, and good industrial development value

Active Publication Date: 2021-05-04
SHANGHAI NEW HUALIAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing chemical synthesis process of prednisolone valerate, the process flow is difficult to grasp, the pure product generated has low purity, complex production process, low production efficiency and high cost, and is not suitable for large-scale production

Method used

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  • Chemical Synthesis Process of Prednisolone Acetate Valerate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1 prednisolone acetate valerate chemical synthesis technique

[0050] Prednisolone valerate chemical synthesis technique, concrete steps are as follows:

[0051] S1: Add 20g of prednisolone to the reaction bottle, control the reaction temperature at 25°C, then add 25ml of a mixed solvent of dichloromethane and dimethyl sulfoxide with a volume ratio of 4:1, stir until the material is dissolved, and obtain Dissolve the system and turn on the nitrogen protection.

[0052]S2: Add 0.5 g of p-toluenesulfonic acid to the solution system in step S1, then add 30 mL of trimethyl orthovalerate, control the reaction temperature at 25°C, stir for 1 hour, and detect the content of prednisolone in the reaction system ≤1wt%, that is, the reaction is complete, and a reaction system containing cyclic esters is obtained.

[0053] S3: Reduce the temperature of the reaction system in step S2 to 20±2°C, add 3mL dilute sulfuric acid solution, then add 20mL acetone, control the re...

Embodiment 2

[0058] Embodiment 2, prednisolone acetate valerate chemical synthesis technique

[0059] Prednisolone valerate chemical synthesis technique, concrete steps are as follows:

[0060] S1: Add 20g of prednisolone to the reaction bottle, control the reaction temperature at 30°C, then add 20ml of dichloromethane and dimethyl sulfoxide with a volume ratio of 8:1, and stir until the material is dissolved to obtain a dissolved system , turn on the nitrogen protection.

[0061] S2: Add 0.6g of p-toluenesulfonic acid to the solution system of step S1, then add 32mL of trimethyl orthovalerate, control the reaction temperature at 30°C, and stir for 1 hour to detect the prednisolone in the reaction system The content of ≤1wt%, that is, the reaction is complete, and the reaction system containing the cyclic ester (II) is obtained.

[0062] S3: Reduce the reaction temperature of the reaction system in step S2 to 20±2°C, add 4mL of dilute sulfuric acid solution, and then add 22mL of acetone,...

Embodiment 3

[0067] Embodiment 3, prednisolone acetate valerate chemical synthesis technique

[0068] Prednisolone valerate chemical synthesis technique, concrete steps are as follows:

[0069] S1: Add 20g of prednisolone to the reaction bottle, control the reaction temperature at 20°C, then add 22ml of dichloromethane and dimethyl sulfoxide with a volume ratio of 6:1, and stir until the material is dissolved to obtain a dissolved system , turn on the nitrogen protection.

[0070] S2: Add 0.8g of p-toluenesulfonic acid to the solution system of step S1, then add 35mL of trimethyl orthovalerate, control the reaction temperature at 20°C, stir and react for 2 hours, and detect the content of prednisolone in the reaction system ≤1wt%, that is, the reaction is complete, and a reaction system containing cyclic esters is obtained.

[0071] S3: Reduce the reaction temperature of the reaction system in step S2 to 20±2°C, add 5mL of dilute sulfuric acid solution, then add 25mL of acetone, control ...

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Abstract

The invention belongs to the technical field of chemical synthesis, and discloses a chemical synthesis process of prednisolone acetate valerate, using prednisolone, p-toluenesulfonic acid, trimethyl orthovalerate, dimethylaminopyridine, pyridine and acetic anhydride as raw materials, and synthesized prednisolone acetate valerate through fewer process steps, which not only simplifies the production process, significantly reduces the production cost, but also has high yield and product purity, and is suitable for large-scale production in factories , has good industrial development value and good market application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a chemical synthesis process of prednisolone valerate. Background technique [0002] As an adrenocortical hormone, prednisolone acetate valerate exhibits excellent anti-inflammatory effects on the affected area, and can also be converted into a highly safe low-active substance in the body, and is widely used for eczema, dermatitis, macule, and insect bites , Itching, prickly heat, hives and other therapeutic agents. In the existing chemical synthesis process of prednisolone acetate valerate, the process flow is difficult to grasp, the pure product generated has low purity, complex production process, low production efficiency and high cost, and is not suitable for large-scale production. For this reason, need to develop the chemical synthesis technique of new prednisolone acetate valerate, to solve the above problems. Contents of the invention [0003] The purpose ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J5/00
CPCC07J5/0053
Inventor 汪武训戚兴凯李游华吉涛
Owner SHANGHAI NEW HUALIAN PHARMA
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