Synthetic method for ethisterone

A synthesis method and a progestogen technology are applied in the directions of steroids, organic chemistry, etc., can solve the problems of increased labor cost, increased progesterone synthesis cost, etc., and achieve the effects of simple operation, solving incomplete reaction, and improving catalytic efficiency.

Inactive Publication Date: 2015-10-28
BAOJI KANGLE BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the increasing shortage of resources such as pycnogenol and turmeric, coupled with the increase in labor costs, has led to a linear upward

Method used

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  • Synthetic method for ethisterone
  • Synthetic method for ethisterone
  • Synthetic method for ethisterone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1. Add 70L of absolute ethanol and 66kg of 4-androstenedione to a clean 200L etherification kettle. After stirring evenly, add 41L of triethyl orthoformate and 1.12kg of pyridine hydrobromide into the etherification kettle After the temperature was raised to 40°C, the etherification reaction was carried out under heat preservation and stirring for 3.5 hours, and there was no raw material point for sampling chromatography. After the reaction material after the etherification reaction was cooled to room temperature, 1.98 L of triethylamine was added to the reaction material, stirred and neutralized The pH value of the final reaction material is 7, and then the reaction material with a pH value of 7 is cooled to below 5°C, and the crystals are obtained by filtration, and the crystals are washed with a mixed solution of triethylamine and absolute ethanol. Dry below ℃ to constant weight to obtain 65kg ether compound I with a yield of 98.48%; the volume percentage of trie...

Embodiment 2

[0036]Step 1. Add 70L of absolute ethanol and 66kg of 4-androstenedione to a clean 200L etherification kettle, stir evenly, and then add 38L of triethyl orthoformate and 0.99kg of pyridine hydrobromide into the etherification kettle After the temperature was raised to 35°C, the etherification reaction was carried out under heat preservation and stirring for 5 hours, and there was no raw material point for sampling chromatography. After the reaction material after the etherification reaction was cooled to room temperature, 1.75L triethylamine was added to the reaction material, and after stirring and neutralization The pH value of the reaction material is 6, and then the reaction material with a pH value of 6 is cooled to below 5°C, and the crystals are obtained by filtration, the crystals are washed with a mixed solution of triethylamine and absolute ethanol, and after drying, the Following drying to constant weight, 64.5kg ether compound I was obtained with a yield of 97.73%; ...

Embodiment 3

[0044] Step 1. Add 70L of absolute ethanol and 66kg of 4-androstenedione to a clean 200L etherification kettle, stir well, and then add 46L of triethyl orthoformate and 1.98kg of pyridine hydrobromide into the etherification kettle After the temperature was raised to 45°C, the etherification reaction was carried out under the condition of heat preservation and stirring for 3 hours, and there was no raw material point for sampling chromatography. After the reaction material after the etherification reaction was cooled to room temperature, 2.12L triethylamine was added to the reaction material, and after neutralization by stirring The pH value of the reaction material is 8, and then the reaction material with a pH value of 8 is cooled to below 5°C, and the crystals are obtained by filtration, and the crystals are washed with a mixed solution of triethylamine and absolute ethanol, and after being dried, they are stored at 80°C Following drying to constant weight, 64.8kg ether comp...

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Abstract

The invention discloses a synthetic method for ethisterone. The synthetic method comprises the following steps that firstly, 4-androstenedione and triethyl orthoformate serve as reaction raw materials, an etherification reaction is conducted, triethylamine is added to adjust the pH value of reaction materials, a crystal is obtained through filtering after cooling, and etherate I is obtained after washing and drying; secondly, dehydration is conducted after methylbenzene, potassium hydroxide and isobutanol are evenly mixed, tetrahydrofuran is added into dehydrated mixed liquid, and acetylene gas is led in until the acetylene gas is not absorbed; thirdly, the dissolved etherate I is added into the mixed liquid, the acetylene gas is led in for a reaction, and sulfuric acid is added until the pH value reaches 1-2; fourthly, the material obtained after the pH value is adjusted is distilled and concentrated, then the distilled and concentrated material is washed to be neutral through water, and an ethisterone crude product is obtained after drying; fifthly, the ethisterone crude product is refined. The synthetic method for the ethisterone has the advantages that reaction conditions are moderate, operation is simple and convenient, reaction steps are few, reaction products are single, and the yield is high. The synthetic method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing progesterone. Background technique [0002] Pregnant itself is a progesterone drug included in the Chinese Pharmacopoeia, and it is also an intermediate raw material for the synthesis of some high-end products. The traditional process uses dienolone acetate as the raw material, which is hydrolyzed through ketoxime reaction and Belleville reaction to obtain important The intermediate --- dehydroepiandrosterone acetate, and then get the crude product of pregnantin through ethynylation reaction and Woshi oxidation reaction, and obtain the fine product after refining and decolorization. In this technique, the synthesis equipment is complicated, the raw material is expensive, the route is complicated, and the yield is low (46.8% based on dienolone acetate). [0003] The dienolone acetate used is obtained by extracting diosgenin from di...

Claims

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Application Information

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IPC IPC(8): C07J1/00
CPCC07J1/0011
Inventor 史永平
Owner BAOJI KANGLE BIOTECH
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