Refining method of hydrocortisone acetate

A technology of hydrocortisone acetate and a refining method, which is applied in organic chemistry, steroid compounds, etc., can solve the problems of cumbersome operation procedures, high production costs, and large environmental pollution, and achieve stable process, simple operation, and simple reaction Effect

Active Publication Date: 2016-08-17
HUNAN NORCHEM PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The operation procedure of this process is cumbersome, the production cost is high due to repeated beating, and the three wastes produced are large, the environmental pollution is large, and the yield is low (about 60%)

Method used

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  • Refining method of hydrocortisone acetate

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Embodiment 1

[0021] A method for refining hydrocortisone acetate of the present invention, comprising the following steps: adding 1 weight part of hydrocortisone acetate crude product, 6 parts by weight of methylene chloride, and 5 parts by weight of methanol to a reactor, heating and refluxing to dissolve Clear, filter, and keep the filter system at 30°C, and feed 0.1 parts by weight of chlorine gas. After the addition, stir for half an hour, concentrate to remove dichloromethane, stop the concentration when the residual amount of methanol reaches 1 part by weight, cool down to 0°C, and centrifuge to obtain the refined product of hydrocortisone acetate. Refined yield: 80.5%, HPLC=99.20%, external standard content: 97.10%, conforming to EP 8.0. The HPLC retention time is consistent with the standard control.

Embodiment 2

[0023] A method for refining hydrocortisone acetate of the present invention, comprising the following steps: adding 1 weight part of hydrocortisone acetate crude product, 8 weight parts of dichloromethane, and 6 weight parts of methanol to a reactor, and heating up to reflux until dissolved Clear, filter, and keep the filtration system at 40°C, then add 0.5 parts by weight of sodium hypochlorite, 0.1 parts by weight of sodium chloride, and then dropwise add glacial acetic acid, the total amount of glacial acetic acid is 0.35 parts by weight. Chloromethane, stop concentrating when the residual amount of methanol reaches 1 weight, cool down to 5°C, and centrifuge to obtain hydrocortisone acetate fine product. Refined yield: 81.5%, HPLC=99.10%, external standard content: 98.10%, conforming to EP 8.0. The HPLC retention time is consistent with the standard control.

Embodiment 3

[0025] A method for refining hydrocortisone acetate of the present invention, comprising the steps of: adding 1 weight part of hydrocortisone acetate crude product, 10 weight parts of dichloromethane, and 4 weight parts of methanol to a reactor, and heating up to reflux until dissolved Clear, filter, keep the filtration system at 35°C, add 0.5 parts by weight of calcium hypochlorite, 0.1 parts by weight of sodium chloride, and then dropwise add glacial acetic acid, the total amount of glacial acetic acid is 0.25 parts by weight, after adding, stir for half an hour, concentrate The dichloromethane was removed, the concentration was stopped when the residual amount of methanol was 1.5 parts by weight, the temperature was lowered to 10° C., and the mixture was centrifuged to obtain the refined product of hydrocortisone acetate. Refined yield: 80.3%, HPLC=99.12%, external standard content: 97.30%, conforming to EP 8.0. The HPLC retention time is consistent with the standard contro...

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Abstract

The invention discloses a refining method for hydrocortisone acetate. The refining method comprises the step of purifying a hydrocortisone acetate crude product with chlorine gas or with hypochorite, glacial acetic acid and sodium chloride, so as to obtain a hydrocortisone acetate refined product. The refining method is simple, convenient, low in manufacturing cost, high in yield and product purity, stable in process, and suitable for producing a large quantity of the hydrocortisone acetate refined product.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy, in particular to a method for refining hydrocortisone acetate. Background technique [0002] Refining hydrocortisone acetate that meets the EP8.0 standard is obtained by beating dichloromethane and chloroform for many times (generally 4 to 8 times) in the current domestic process. The operation procedure of the process is cumbersome, the repeated beating results in high production cost, a lot of three wastes, great environmental pollution, and low yield (about 60%). Therefore, it is urgent to develop a new refining method for hydrocortisone acetate. Contents of the invention [0003] The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art and provide a simple and convenient method for refining hydrocortisone acetate with low production cost, high yield, high product purity, stable process and suitable for mass production. [0004] In order ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J5/00
CPCC07J5/0053
Inventor 刘喜荣曾春玲
Owner HUNAN NORCHEM PHARMACEUTICAL CO LTD
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