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A kind of extraction process of mold oxide

A technology of mold oxide and extraction process, applied in steroids, organic chemistry and other directions, can solve the problems of high production cost and complex extraction process, and achieve the effect of low production cost, simple process and cost saving.

Active Publication Date: 2017-06-06
ANYANG JIUZHOU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide an extraction process of mold oxides, which can overcome the defects of complicated extraction process and high production cost at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A process for extracting mold oxides, mixing the mixture of mold oxides, Wormwood and mycelium with a mixture of toluene and chloroform (the volume ratio of the two is 1:5) (the ratio of the mixture to the mixture is 1 :4), then raise the temperature to 70°C for 25 minutes to fully dissolve, then separate the solid and liquid, and refine and concentrate the filtrate at a temperature of 110°C until the quality of the solid in the concentrate is equivalent to that of the liquid, then cool down to below 30°C, For the second solid-liquid separation, add a mixture of toluene and chloroform to the separated solids again (the ratio is the same as before), repeat the above-mentioned operations of heating up to fully dissolve, solid-liquid separation, filtrate refining and concentration, and secondary solid-liquid separation. The filter cake is the fine product of mold oxides; the filtrate after the second solid-liquid separation is used for the recovery of Wormwood. The operati...

Embodiment 2

[0022] A process for extracting mold oxides, mixing the mixture of mold oxides, Wormwood and mycelium with a mixture of toluene and chloroform (the volume ratio of the two is 1:4) (the ratio of the mixture to the mixture is 1 :3), then raise the temperature to 60°C for 30 minutes to fully dissolve, then separate the solid and liquid, and refine and concentrate the filtrate at a temperature of 110°C until the quality of the solid in the concentrate is equivalent to that of the liquid, and then lower the temperature below 30°C for the second time For solid-liquid separation, add a mixture of toluene and chloroform to the separated solids, repeat the above-mentioned operations of heating up to fully dissolve, solid-liquid separation, filtrate refining and concentration, and secondary solid-liquid separation. The separated filter cake is mold oxidation. The product is fine; the filtrate after the second solid-liquid separation is used for the recovery of Woshi's product. A total o...

Embodiment 3

[0025] A process for extracting mold oxides, mixing the mixture of mold oxides, Wormwood and mycelium with a mixture of toluene and chloroform (the volume ratio of the two is 1:6) (the ratio of the mixture to the mixture is 1 :5), then raise the temperature to 80°C for 20 minutes to fully dissolve, then separate the solid and liquid, and refine and concentrate the filtrate at a temperature of 120°C until the solids in the concentrate are equivalent to the liquid quality, then lower the temperature below 30°C, for the second time For solid-liquid separation, add a mixture of toluene and chloroform to the separated solids, repeat the above-mentioned operations of heating up to fully dissolve, solid-liquid separation, filtrate refining and concentration, and secondary solid-liquid separation. The separated filter cake is mold oxidation. The product is fine; the filtrate after the second solid-liquid separation is used for the recovery of Woshi's product. A total of 5 operations o...

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Abstract

The invention belongs to the technical field of medical intermediate synthesis and in particular relates to an extraction process of 11a-hydroxy-16,17a-epoxyprogesterone. The extraction process is characterized by mixing a mixture of 11a-hydroxy-16,17a-epoxyprogesterone, methoxydienone and mycelia with mixed liquor of toluene and chloroform, then raising the temperature to fully dissolve the mixture, then carrying out solid-liquid separation, refining and concentrating the filtrate, carrying out secondary solid-liquid separation, adding the mixed liquor of toluene and chloroform to a solid matter obtained by separation, and repeating the operations of raising the temperature to fully dissolve the mixture, carrying out solid-liquid separation, refining and concentrating the filtrate and carrying out secondary solid-liquid separation, thus obtaining a filter cake after separation, namely the refined 11a-hydroxy-16,17a-epoxyprogesterone product. The extraction process has the advantages of concise flow, low equipment requirements, low production cost and little environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, in particular to a process for extracting fungal oxides. Background technique [0002] The Chinese name of mold oxide is 11a-hydroxy-16,17a-epoxyprogesterone, molecular formula: C 21 h 28 o 4 , molecular weight: 344.44. It is an intermediate of cortisone acetate and fluocinolone acetate. Its common preparation method is to prepare diosgenin through ring-opening, acetylation, oxidation, hydrolysis, elimination, epoxidation, oxidation and other steps. The extraction of mold oxides mainly refers to the extraction of mold oxides from the mixture of mold oxides, Wormwood and other impurities such as mycelia. The existing method is to extract with acetone, and then refine with toluene and chloroform. The principle is to use acetone to extract mold oxides and Wormwood, to achieve the purpose of separation of materials and mycelia. Then, according to the different...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
Inventor 曹俊华
Owner ANYANG JIUZHOU PHARMA