Triamcinolone preparation method

A compound and organic solvent technology, applied in the field of preparation of triamcinolone, can solve the problems of cumbersome product purification, and achieve the effects of excellent yield and cost, high yield and good quality

Inactive Publication Date: 2019-02-01
SHANDONG TAIHUA BIO & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to provide a preparation method of triamcinolone, which overcomes the problem of complicated product purification caused by by-products in the existing preparation process of triamcinolone

Method used

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Embodiment 1

[0031] The preparation method of the triamcinolone involved in this embodiment specifically comprises the following steps:

[0032] (1) Oxidation reaction: Add 30g of the compound of formula I and 30ml of formic acid into 600ml of methanol at a temperature of -10°C, and carry out the oxidation reaction under the action of excess potassium permanganate. After the TLC test is qualified, add excess sodium bisulfite Remove the acid and oxidizing agent from the aqueous solution, then concentrate, add water to precipitate the product, control the temperature during the precipitation process below 5°C, finally centrifuge the material, and dry to obtain 30.3g of the compound of formula II, with a yield of 101%;

[0033] (2) Esterification reaction: Add 30.3g of the compound of formula II obtained in step (1) into 303ml of chloroform, carry out esterification reaction with 30.3ml of acetic anhydride, heat and reflux with steam for 14-16 hours, and TLC detects that there is no raw materi...

Embodiment 2

[0040] The preparation method of the triamcinolone involved in this embodiment specifically comprises the following steps:

[0041] (1) Oxidation reaction: Add 30g of formula I compound and 60ml perchloric acid into 1200ml of dichloromethane at -5°C, carry out oxidation reaction under the action of excess potassium dichromate, after TLC detection is qualified, add excess sodium sulfite Remove the acid and oxidizing agent from the aqueous solution, then concentrate, add water to precipitate the product, control the temperature during the precipitation process below 5°C, finally centrifuge the material, and dry to obtain 30 g of the compound of formula II, with a yield of 100%;

[0042] (2) Esterification reaction: add 30g of the compound of formula II obtained in step (1) into 300ml of dichloromethane, carry out esterification reaction with 30ml of acetic acid, heat and reflux with steam for 14-16 hours, the end of the reaction when there is no raw material point detected by TLC...

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Abstract

The invention discloses a triamcinolone preparation method, and belongs to the technical field of pharmacy. The triamcinolone preparation method comprises: selecting a tetraenyl acetate material as araw material, carrying out oxidation, esterification at 16 site, epoxidation and fluorination, and hydrolyzing after the fluorination refining to obtain triamcinolone. According to the present invention, the yield and the cost of the method of the present invention are obviously superior to the synthesis method sequentially comprising oxidation and direct epoxidation, wherein the impurity is removed after the fluorination process, such that the problem that the impurity is difficultly removed in the final refining can be avoided, and the impurity can be controlled at the intermediate stage soas to reduce the difficulty in the separation and purification.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a preparation method of triamcinolone. It firstly selects tetraenyl acetate as a raw material, and then undergoes oxidation, 16-position ester, epoxy, fluorine, and fluorine, and then hydrolyzes to obtain triamcinolone at last. Background technique [0002] Triamcinolone is an adrenal corticosteroid and adrenocorticotropic hormone drug. Its anti-inflammatory effect is stronger than that of hydrocortisone and prednisone, and its water and sodium retention effect is relatively mild. It is suitable for rheumatoid arthritis and other diseases. Connective tissue diseases, etc., especially suitable for arthritis patients with high blood pressure or edema who are contraindicated for corticosteroids. At present, there are many preparation techniques for triamcinolone, most of which use tetraenyl acetate as raw materials. Patent CN107793461A adopts the following synthetic r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J3/00
CPCC07J3/005
Inventor 王京沪
Owner SHANDONG TAIHUA BIO & TECH
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