Dehydropregnenolone acetate extraction process

A technology of dienool ketone acetate and extraction process, which is applied in the directions of steroids, organic chemistry, organic chemistry methods, etc., can solve the problems of violent reaction in oxidation mode, difficult to handle pollution of intermediates, etc., so as to save extraction cost, The effect of reducing extraction cost and easy control

Pending Publication Date: 2021-04-06
湖北民生生物医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the deficiencies in the prior art, the invention provides a dienolone acetate extraction process, which has the advantages of good environmental protection effect, and solves the problem that the existing dienolone acetate process usually uses chromium trioxide and other substances as Oxidants are used to complete the oxidation reaction. However, this oxidation method reacts violently, and the intermediates produced are difficult to handle and highly polluting.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment one: a kind of dienolone acetate extraction process, comprises the following steps:

[0024] 1) Take 5 parts of acetic anhydride and 10 parts of acetic acid for mixing, and put 10 parts of preferred saponin into the mixed solution of acetic anhydride and acetic acid, and heat to reflux for 1 hour to obtain a ring-opening mixed solution;

[0025] 2) Cool the ring-opening mixed solution in step 1) to 45° C., add 2 parts of oxidizing agent for oxidation reaction, and react under stirring for 1 hour to obtain the mixed solution of oxide;

[0026] 3) Add 2 parts of impurity remover to the oxide mixture in step 2), and stir for 0.5 hours, then add an appropriate amount of water and heat for hydrolysis for 1 hour to obtain a hydrolysis solution;

[0027] 4) Adding 15 parts of hexahydrobenzene to the hydrolysis solution in step 3) for extraction and liquid separation to obtain a residue, adding part of ethanol to the residue and heating and dissolving to obtain a sol...

Embodiment 2

[0029] Embodiment two: a kind of dienolone acetate extraction process, comprises the following steps:

[0030] 1) Take 10 parts of acetic anhydride and 20 parts of acetic acid for mixing, and put 20 parts of preferred saponins into the mixed solution of acetic anhydride and acetic acid, and heat to reflux for 2 hours to obtain a ring-opening mixed solution;

[0031] 2) Cool the ring-opening mixed solution in step 1) to 45° C., add 4 parts of oxidant for oxidation reaction, and react for 2 hours under stirring to obtain the mixed solution of oxide;

[0032] 3) Add 4 parts of impurity remover to the oxide mixture in step 2), and stir for 1 hour, then add an appropriate amount of water and heat for hydrolysis for 2 hours to obtain a hydrolysis solution;

[0033] 4) adding 20 parts of hexahydrobenzene to the hydrolysis solution in step 3) for extraction and liquid separation to obtain a residue, adding 10 parts of ethanol to the residue and heating and dissolving to obtain a solut...

Embodiment 3

[0035] Embodiment three: a kind of dienolone acetate extraction process, comprises the following steps:

[0036] 1) Take 15 parts of acetic anhydride and 30 parts of acetic acid for mixing, and put 30 parts of preferred saponins into the mixed solution of acetic anhydride and acetic acid, and heat to reflux for 3 hours to obtain a ring-opening mixed solution;

[0037] 2) Cool the ring-opening mixed solution in step 1) to 45° C., add 6 parts of oxidizing agent to carry out oxidation reaction, and react under stirring for 3 hours to obtain the mixed solution of oxide;

[0038] 3) Add 6 parts of impurity remover to the oxide mixture in step 2), and stir for 1.5 hours, then add an appropriate amount of water and heat for hydrolysis for 3 hours to obtain a hydrolysis solution;

[0039] 4) adding 25 parts of hexahydrobenzene to the hydrolysis solution in step 3) for extraction and liquid separation to obtain a residue, adding 15 parts of ethanol to the residue and heating and dissol...

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PUM

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Abstract

The invention relates to the technical field of dehydropregnenolone acetate extraction, and discloses a dehydropregnenolone acetate extraction process which comprises the following steps: mixing 5-15 parts of acetic anhydride and 10-30 parts of acetic acid, and adding 10-30 parts of saponin into the mixed solution of acetic anhydride and acetic acid. According to the dehydropregnenolone acetate extraction process, acetic anhydride, acetic acid and saponin are subjected to a ring-opening reaction, an obtained solution can be oxidized, then hydrogen peroxide is used for replacing traditional chromium trioxide to serve as an oxidizing agent, the production cost is low, almost no pollution is caused, and redundant hydrogen peroxide is simple to treat; sodium sulfite is only required to be poured to react with hydrogen peroxide to obtain sodium sulfate and water, sodium sulfate can be recycled in a layered manner in the last step of filtration, and compared with the adoption of chromium trioxide as an oxidant, the production cost is low, the pollution is low, the obtained product can be recycled, and the reaction process is relatively mild and easy to control; and the purpose of good environmental protection is achieved.

Description

technical field [0001] The invention relates to the technical field of dienolone acetate extraction, in particular to a dienolone acetate extraction process. Background technique [0002] Dienolone acetate is an important intermediate in the synthesis of steroid hormone APIs. It can be used as a raw material to produce adrenal hormone drugs, glucocorticoid drugs, steroidal anti-inflammatory drugs, sex hormone drugs and female oral contraceptives medicine etc. [0003] At present, there are various techniques for extracting dienolone acetate on the market, but there are generally disadvantages of poor environmental protection effect. The existing techniques for dienolone acetate usually use materials such as chromium trioxide as oxidant The oxidation reaction is completed, but this oxidation method reacts violently, and the intermediates produced are difficult to handle and highly polluting. Therefore, a dienolone acetate extraction process is proposed to solve the above-men...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J13/00
CPCC07J13/005C07B2200/13
Inventor 陈孝华邓海锋张兴军
Owner 湖北民生生物医药有限公司
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