Process method for producing intermediate 3,20-diethylene glycol of betamethasone serial products

A series of products, the technology of betamethasone, applied in the field of chemical medicine, can solve the problems of serious equipment loss and energy consumption, unsatisfactory condensate quality, and great human poisoning, so as to reduce equipment loss, shorten reaction time, and reduce harm and the effect of environmental pollution

Inactive Publication Date: 2009-10-21
HENAN LIHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is necessary to use benzene, which is highly toxic to the human body and seriously pollutes the environment, as a solvent. It is prepared under high temperature and high speed production conditions for a long time by reflux reaction, which is quite serious for equipment loss and energy consumption.
And the product yield is low, and the quality situation of the condensate is also unsatisfactory

Method used

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  • Process method for producing intermediate 3,20-diethylene glycol of betamethasone serial products
  • Process method for producing intermediate 3,20-diethylene glycol of betamethasone serial products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Example 1: Comparative example, traditional preparation process

[0010] Using the existing production process for preparing the condensate of betamethasone series products, 70g of cortisone acetate intermediate Platts oxide, 383g of ethylene glycol, and 1218g of benzene were added into the reaction flask, and stirred at 75-80℃ for refluxing and separating water for 1 hour. , Adding 0.7 g of p-toluenesulfonic acid and continuing to stir and reflux at 80°C for 10 hours, and the reaction is complete. It was concentrated under reduced pressure until crystals precipitated, cooled to 10°C, filtered, and dried to obtain 68.5 g of condensate, with an HPLC content of 86%.

Embodiment 2

[0011] Example 2: Process of the present invention

[0012] Add 70g of cortisone acetate intermediate Platts oxide, 196g of ethylene glycol, 80g of triethyl orthoformate, 140g of chloroform, and 1.5g of boron trifluoride-diethyl ether into the reaction flask, and stir to react at 20-25°C. After 5 hours, the reaction was complete. It was concentrated under reduced pressure until crystals precipitated, cooled to 10°C, filtered, and dried to obtain 75 g of a condensate with a HPLC content of 90%.

Embodiment 3

[0013] Example 3: Process of the present invention

[0014] Add 70g of Cortisone acetate intermediate Platts oxide, 196g of ethylene glycol, 80g of triethyl orthoformate, 140g of methylene chloride, and 1.5g of boron trifluoride-diethyl ether into the reaction flask, and stir to react at 20-25°C. After 5 hours, the reaction was complete. It was concentrated under reduced pressure until crystals precipitated, cooled to 10°C, filtered, and dried to obtain 75.3 g of a condensate with an HPLC content of 91%.

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Abstract

The invention discloses a process method for producing an intermediate 3,20-diethylene glycol of betamethasone serial products, which belongs to the field of chemical medicaments. The method comprises the following steps: using a cortisone acetate intermediate prowazekii oxide (1) and glycol as raw materials, boron trifluoride and triethyl orthoformate as catalysts, and chloralkane as a menstruum to perform reaction; and concentrating, crystallizing, filtering, washing and drying the reactants to obtain a reaction product. The method can increase the batch charging concentration, shorten the reaction time, and greatly improve the yield and the quality of a condensation compound. Besides, the method reduces the equipment loss, avoids the use of benzene solvents which are more harmful, and greatly reduces the harm to health and the pollution to the environment.

Description

1. Technical Field: [0001] The invention relates to a production process of a betamethasone series product, in particular to a production process of a betamethasone series product 3,20 diethylene glycol, and belongs to the field of chemical medicine. 2. Background technology: [0002] The traditional production method for preparing betamethasone series product 3,20 double ethylene glycol intermediate is: use cortisone acetate intermediate Platts oxide as raw material, stir together with benzene and ethylene glycol, and azeotropically distill to remove water. , Adding p-toluenesulfonic acid, refluxing reaction at 80°C for 10 hours, cooling, and recovering benzene and ethylene glycol by distillation under reduced pressure to precipitate crystals to obtain 3,20 diethylene glycol intermediate. It is necessary to use benzene, which is highly toxic to human body and seriously pollute the environment, as a solvent, and it is prepared by reflux reaction for a long time under high-tempera...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00B01J31/02B01J27/12
Inventor 段爱朝
Owner HENAN LIHUA PHARMA
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