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Preparation process for deflazacort

A preparation process, the technology of deflazacort, applied in the field of deflazacort preparation process, can solve the problems of high production cost, complicated process operation, difficult sewage treatment, etc., and achieve simple production operation, economical and environmentally friendly process, and product yield. high rate effect

Inactive Publication Date: 2018-09-04
YUEYANG HUANYU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problems raised in the above-mentioned background technology, the object of the present invention is to provide a preparation process of deflazacort, which can significantly reduce its production cost, so as to avoid difficult sewage treatment, complicated process operation and difficult production in the traditional production process of deflazacort. High cost and many other defects

Method used

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  • Preparation process for deflazacort
  • Preparation process for deflazacort
  • Preparation process for deflazacort

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Oxide preparation: Add 95 parts of mold dehydrogenation products, 180 parts of glacial acetic acid, and 35 parts of chromic anhydride to the reaction kettle, stir and react for 4 to 5 hours at a temperature of 35-38°C, and add 1700 parts of concentration to the water analysis kettle 5% caustic soda aqueous solution for water analysis, centrifugation and filtration to obtain oxides.

[0024] Preparation of protective material: add 90 parts of oxides, 40-60 parts of glacial acetic acid, 1500 parts of water, 35 parts of methyl carbazate in the reaction kettle, react for 10 hours at a temperature of 20-25 ° C, and centrifugally filter to obtain protection. thing.

[0025] Preparation of closed-loop hydrolyzate: Add 120 parts of protective materials and 750 parts of chloroform into the reaction kettle, stir, control the temperature at 25-28°C, feed nitrogen, keep warm for 24-30 hours, and after the reaction is complete, pump the materials into the washing kettle. Add water ...

Embodiment 2

[0029] Preparation of oxides: Add 90 parts of mold dehydrogenation products, 200 parts of glacial acetic acid, and 30 parts of chromic anhydride into the reaction kettle, stir and react for 4 to 5 hours at a temperature of 35-38°C, and add 1600 parts of concentration to the water analysis kettle 5% caustic soda aqueous solution for water analysis, centrifugation and filtration to obtain oxides.

[0030] Preservation preparation: Add 90 parts of oxides, 50 parts of glacial acetic acid, 1600 parts of water, 40 parts of methyl carbazate into a reaction kettle, react at 20-25°C for 10 hours, and centrifuge to obtain the protection.

[0031] Preparation of closed-loop hydrolyzate: Add 120 parts of protective material and 800 parts of chloroform into the reaction kettle, stir, control the temperature at 25-28°C, feed nitrogen gas, keep warm for 24-30 hours, and after the reaction is complete, pump the material into the washing kettle. Add water to wash once, dry chloroform under neg...

Embodiment 3

[0035] Preparation of oxides: add 110 parts of mold dehydrogenation products, 240 parts of glacial acetic acid, and 40 parts of chromic anhydride in the reaction kettle, stir and react for 4 to 5 hours at a temperature of 35-38°C, and add 1900 parts of concentration in the water analysis kettle 5% caustic soda aqueous solution for water analysis, centrifugation and filtration to obtain oxides.

[0036] Preservation preparation: add 95 parts of oxides, 60 parts of glacial acetic acid, 1900 parts of water, 50 parts of methyl carbazate in a reaction kettle, react at a temperature of 20-25°C for 10 hours, and centrifuge to obtain the protection.

[0037]Preparation of closed-loop hydrolyzate: Add 130 parts of protective material and 900 parts of chloroform into the reaction kettle, stir, control the temperature at 25-28°C, feed nitrogen, keep warm for 24-30 hours, and after the reaction is complete, pump the material into the washing kettle. Add water to wash once, dry the chlorof...

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Abstract

The invention relates to a preparation process for deflazacort. The process comprises the following steps: preparation of an oxide; preparation of a protective substance; preparation of a closed-loophydrolyzate; an iodination reaction; and a replacement reaction. The process provided by the invention can significantly reduce production costs, and avoid a plurality of defects that sewage treatmentis difficult, process operation is complicated and the production costs are high in a traditional production process of the deflazacort.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a preparation process of deflazacort. Background technique [0002] Deflazacort is mainly used as corticosteroid pharmaceutical raw materials and intermediates. It is a white or off-white crystalline powder with anti-inflammatory and anti-allergic effects, which is 10 to 20 times equivalent to prednisolone. It is used for adrenal cortex function Hypothyroidism, autoimmune diseases, allergic diseases and blood system diseases, etc., during the production of traditional deflazacort, multi-step chemical reactions are required for production, so the raw material consumption is high, resulting in the production cost of deflazacort and the market price. The substantial growth has had a major impact on the global market of deflazacort drugs, and more waste water is produced, which is difficult to treat and easily pollutes environmental water. Contents of the invention ...

Claims

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Application Information

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IPC IPC(8): C07J71/00
CPCC07J71/0068
Inventor 徐润星
Owner YUEYANG HUANYU PHARMA
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