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Preparation method of steroid intermediate

A technology for intermediates and steroids, applied in the field of pine preparation, can solve problems such as containing heavy heavy metal ions, and achieve the effects of low price, mild reaction conditions and good process prospects

Active Publication Date: 2018-08-07
JIANGSU YUANDA XIANLE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a new synthetic route of steroidal intermediate cortisone acetate, avoid the use of heavy metal raw materials, solve the problem of a large amount of heavy metal ions in the waste water from the source, and solve one of the above-mentioned prior art problems or more

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Steroid intermediate A

[0041] Add 20 parts by volume of acetone to the dry first reaction tank, feed nitrogen, stir and add 1 part by mass of 17α-hydroxypregna-4,9-diene-3,20-dione acetate, stir After 15 minutes, cool down to 0-5°C, add 0.06 parts by volume of perchloric acid and 2 parts by volume of water, add 0.5 parts by mass of dibromohydantoin four times at 2-4°C, with an interval of 30 minutes each time, After the addition is completed, keep the temperature for 2 hours, and take a sample for detection and analysis by thin-layer chromatography until the raw materials are completely reacted;

[0042] After completion of the reaction, add dropwise a concentration of 10% sodium sulfite aqueous solution to the reaction solution to adjust the pH>7. For the distillate, add 2 parts by volume of water, and then steam until there is no acetone smell, that is, the concentration is complete;

[0043] Add 25 parts by volume of water, stir and cool down to 0-5°C, discha...

Embodiment 2

[0053] (1) Steroid intermediate A

[0054]Add 15 parts by volume of acetone to the dry first reaction tank, feed nitrogen, stir and add 0.8 parts by mass of 17α-hydroxypregna-4,9-diene-3,20-dione acetate, stir After 15 minutes, cool down to 0-5°C, add 0.04 parts by volume of perchloric acid and 1 part by volume of water, add 0.4 parts by mass of dibromohydantoin four times at 2-4°C, with an interval of 30 minutes each time, After the addition is completed, keep the temperature for 1 hour, and take a sample and analyze it by thin-layer chromatography until the raw material is completely reacted;

[0055] After completion of the reaction, add dropwise concentration of 10% sodium sulfite aqueous solution to the reaction solution to adjust pH>7. For the distillate, add 2 parts by volume of water, and then steam until there is no acetone smell, that is, the concentration is complete;

[0056] Add 20 parts by volume of water, stir and cool down to 0-5°C, discharge and centrifuge, ...

Embodiment 3

[0065] (1) Steroid intermediate A

[0066] Add 25 parts by volume of acetone to the dry first reaction tank, feed nitrogen, stir and add 1.2 parts by mass of 17α-hydroxypregna-4,9-diene-3,20-dione acetate, stir After 15 minutes, cool down to 0-5°C, add 0.08 parts by volume of perchloric acid and 3 parts by volume of water, add 0.6 parts by mass of dibromohydantoin four times at 2-4°C, with an interval of 30 minutes each time, After the addition is completed, keep the temperature for 3 hours, and take a sample and analyze it by thin-layer chromatography until the raw material is completely reacted;

[0067] After completion of the reaction, add dropwise concentration of 10% sodium sulfite aqueous solution to the reaction solution to adjust the pH>7. For the distillate, add 2 parts by volume of water, and then steam until there is no acetone smell, that is, the concentration is complete;

[0068] Add 30 parts by volume of water, stir and cool down to 0-5°C, discharge and centr...

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Abstract

The invention discloses a preparation method of a steroid intermediate. The preparation method comprises the following steps: adding a first solvent, a first acid solution, water and 17-alpha-hydroxypregnenolone steroid-4,9-diene-3,20-diketone acetate into a first reaction tank, and uniformly stirring; adding a bromination agent in four times at 2-4 DEG C, maintaining the temperature for reactingfor 2h, and carrying out thin-layer chromatography analysis until the reaction of the raw materials is finished; and regulating the pH value to be more than 7, regulating the pH value back to 6, carrying out reduced pressure concentration until the first solvent is completely concentrated, adding water, cooling to 5 DEG C, and carrying out centrifugation, cleaning, spin-drying and drying, so as toobtain the steroid intermediate, namely cortisone. According to the preparation method, an oxidant and a catalyst which contain heavy metal ions are not used, the used solvent can be recycled and reused, wastewater does not contain heavy metal ions in the production process, the method belongs to an environment-friendly process and has very good process prospects, and the yield and purity of theproduct are high.

Description

technical field [0001] The invention relates to the technical field of medicines and intermediates thereof, in particular to a method for preparing an important steroid intermediate cortisone acetate, which can be used as a starting material for cortisone, prednisone, and prednisone Production of APIs of steroid hormones such as Nisolone and Methylprednisolone and related derivatives. Background technique [0002] Steroid hormones have strong anti-infection, anti-allergic, anti-viral and anti-shock pharmacological effects, and are important drugs for treating rheumatism, cardiovascular, lymphoid leukemia, cellular encephalitis, skin diseases, anti-tumor and rescuing critically ill patients. Structurally, it can be divided into androstane, estrone and pregnane. Among them, prednisolone has the third mother nucleus structure, so it belongs to the adrenal cortex hormone drugs with pregnane structure. [0003] Cortisone acetate is an important steroid compound, not only can be...

Claims

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Application Information

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IPC IPC(8): C07J5/00C07J21/00
CPCC07J5/0053C07J21/006
Inventor 郭曦刘年金杜艳赵百合
Owner JIANGSU YUANDA XIANLE PHARMA
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