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A kind of method for preparing 7α-methyl-19-aldehyde group-4-androstene-3,17-dione by electrocatalytic oxidation

A technology for electrocatalytic oxidation and androstene, which is applied in organic chemistry, electrolysis components, electrolysis processes, etc., can solve the problems of polluted environment, long reaction time, low product selectivity, etc., and achieves high product yield, low cost, selective effect

Active Publication Date: 2022-02-15
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above preparation methods all use chemical oxidants, the reaction time is longer, the product selectivity is low, and there are problems such as environmental pollution.

Method used

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  • A kind of method for preparing 7α-methyl-19-aldehyde group-4-androstene-3,17-dione by electrocatalytic oxidation
  • A kind of method for preparing 7α-methyl-19-aldehyde group-4-androstene-3,17-dione by electrocatalytic oxidation
  • A kind of method for preparing 7α-methyl-19-aldehyde group-4-androstene-3,17-dione by electrocatalytic oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: Synthesis of NiO / CF Catalyst and its electrocatalytic oxidation 7α-methyl-17, 19-dihydroxy-4-α-methyl-19-aldehyde-4-4- Hernene-3,17-diketone

[0032](1) According to the press, 581 mg of nickel nitrate is dissolved in 80 mL distilled water, then 480 mg of urea and 296 mg of ammonium fluoride, and the solution is ultrasonically dispersed for 30 minutes to obtain a precursor solution A;

[0033] (2) Add the solution A and the carbon fabric in step 1) to the hydrothermal kettle, 12 hours in 120 ° C for 12 hours, then cool, remove the carbon cloth carrier, then washed three times with distilled water and ethanol, then placed The load type catalyst was dried in a vacuum drying tank at 60 ° C;

[0034] (3) Step 2) The dried load type catalyst is placed in a tube furnace, and 600 ° C is calcined at 600 ° C for 2 hours under the air atmosphere, i.e., obtaining the load type nickel oxide catalyst, labeled NIO / CF, SEM scanning electron microscopy figure 1 and 2 Indicat...

Embodiment 2

[0040] Example 2: Synthesis of COO / CF Catalyst and Its Electrocatalytic Oxidation 7α-Methyl-17, 19-Dihydroxy-4-Trobe-3-ketogenesis 7α-methyl-19-aldehyde-4- Hernene-3,17-diketone

[0041] (1) According to the press, 258 mg of cobalt chloride is dissolved in 40 mL distilled water, and then 240 mg of urea and 74 mg of ammonium fluoride, the solution is ultrasonically dispersed for 30 minutes to obtain a precursor solution A;

[0042] (2) Add the solution A and the carbon cloth in step 1 to the hydrothermal kettle, and the heat is 10 hours at 100 ° C, and the reaction is cooled, and the carbon cloth carrier is removed, then washed three times with distilled water and ethanol, then placed The load type catalyst was dried in a vacuum drying tank at 60 ° C;

[0043] (3) Step 2) The load-bearing catalyst was placed in a tubular furnace and calcined at 400 ° C under an air atmosphere for 2 hours, i.e., cooled to room temperature, i.e., to obtain a cobalt oxide catalyst, labeled COO / CF....

Embodiment 3

[0049] Example 3: Fe 2 O 3 Synthesis of cf catalyst and its electrocatalytic oxidation 7α-methyl-17, 19-dihydroxy-4-α-methyl-19-aldehyde-4-α-methyl-19-aldehyde-4-α -3-3 , 17-diketa

[0050] (1) According to the press, 726 mg of iron-soluble water was taken in 60 mL distilled water, and then 720 mg of urea and 222 mg of ammonium fluorinated ammonium fluoride, and the solution was ultrasonically dispersed for 30 minutes to obtain a precursor solution A;

[0051] (2) The solution A and the carbon cloth in step 1 are added to the hydrothermal kettle, and the hot reaction at 140 ° C for 6 hours, then cooled, then the carbon cloth carrier was removed, then washed three times with distilled water and ethanol, then placed The load type catalyst was dried in a vacuum drying tank at 60 ° C;

[0052] (3) Step 2) After drying the load type catalyst is placed in a tube furnace, calcined by 500 ° C for 1 hour under the air atmosphere, which is cooled to room temperature, i.e., obtaining the loa...

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Abstract

The invention relates to a method for preparing 7α-methyl-19-aldehyde group-4-androstene-3,17-dione by electrocatalytic oxidation, specifically: using an H-type electrolytic cell for the reaction, in the anode chamber, The metal oxide catalyst is used as a working electrode, and 7α-methyl-17,19-dihydroxy-4-androstene-3-one is used as a reaction substrate dissolved in a mixed solvent as an anolyte, and nitrogen oxide free radicals are added As a medium; in the cathode chamber, the platinum sheet is used as the counter electrode, and the weak alkaline solution is used as the catholyte, and the electrocatalytic oxidation reaction is carried out in a constant temperature water bath. After the reaction is completed, an organic solvent is added for extraction to obtain an organic extract. This gives 7α-methyl-19-aldehyde-4-androstene-3,17-dione. The condition of the electrocatalytic oxidation reaction process of the present invention is mild, green and pollution-free, the conversion rate of raw materials is high, the selectivity of 7α-methyl-19-aldehyde group-4-androstene-3,17-dione is good, and the yield is high , Compared with noble metal catalysts, the transition metal oxide catalysts used in the present invention have low cost and avoid the consumption of rare and noble metals.

Description

Technical field [0001] The present invention relates to a synthetic method of steroidal hormone drug product, belonging to the field of fine chemical production, and in particular, to electrocatalytic oxidation, 7α-methyl-19-aldehyde-4-α-3,17- Method of diketone. Background technique [0002] 7α-methyl-19-aldehyde-4-α-3,17-dikone is a key intermediate of high-efficiency steroid hormone such as synthetic Mibaron, Budron. Miblon, the Bron Ronal product has pregnancy, estrogen and androgen activity, in the treatment of women's menopausal syndrome, prevents women with postmenopausal bone loss. In 1986, NP Van Vleit et al. Reported a Jones agent as an oxidant, oxidized synthesis of 7α-methyl-19-aldehyde-4-α-3,17-diketone method, but the oxidant The 19-position hydroxyl group was oxidized into a carboxylic acid during the reaction, about 8% of the raw material, and the yield of the referral reported that the yield was only about 60%, and the yield was to be improved (RECL. TRAV. Chim. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/23C25B3/07
CPCC07J1/0011C07J1/0022C07J1/0018
Inventor 王建国李随勤钟兴贺佳辉
Owner ZHEJIANG UNIV OF TECH
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