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Synthesis method of betamethasone epoxy hydrolyzate

A technology of betamethasone and synthetic methods, applied in the direction of steroids, organic chemistry, etc., can solve the problems of product yield loss, hydrolysis run-off, etc., and achieve low production costs, reduced hydrolysis, and reduced raw and auxiliary materials and power costs Effect

Active Publication Date: 2015-09-30
ZHEJIANG XIANJU XIANLE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The main problems of this synthesis process route are: in the post-treatment of betamethasone esterification reaction in this process, the hydrolyzed part runs out during water analysis, which leads to the loss of product yield, and betamethasone bromide can be directly synthesized by hydrolysis of epoxy thing
According to theoretical yield, and from the yield (about 65%) of this betamethasone epoxy hydrolyzate process, the yield of betamethasone epoxy hydrolyzate still has room to improve

Method used

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  • Synthesis method of betamethasone epoxy hydrolyzate
  • Synthesis method of betamethasone epoxy hydrolyzate
  • Synthesis method of betamethasone epoxy hydrolyzate

Examples

Experimental program
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Effect test

Embodiment 1

[0050] A kind of synthetic method of betamethasone epoxy hydrolyzate, comprises the steps:

[0051] (1) take betamethasone digest as raw material, prepare betamethasone bromide through bromohydroxylation reaction, and the reaction process is:

[0052] Add 118L of dioxane and 32kg of betamethasone to a dry bromohydrin reaction tank, blow nitrogen gas, and stir until it dissolves; control the temperature between 10 and 18°C, slowly add 4.1L of perchloric acid, and control When the temperature is between 10 and 20°C, add 18.24kg of beta 101 (i.e. N-bromosuccinimide), after the addition, keep it at 10°C for 40 minutes, then add 104L of methanol and stir for 8 minutes; Pull the reaction solution into the existing sodium sulfite solution (dissolve 7-7.36kg of sodium sulfite in 40L of water) and 1344L of water at an internal temperature of 5-10°C for water analysis in a bromine water analysis tank, and control the water analysis temperature at 5-20°C Between (use starch-potassium io...

Embodiment 2

[0057] A kind of synthetic method of betamethasone epoxy hydrolyzate, comprises the steps:

[0058] (1) take betamethasone digest as raw material, prepare betamethasone bromide through bromohydroxylation reaction, and the reaction process is:

[0059] Add 115L of dioxane and 32kg of betamethasone to the dry bromohydrin reaction tank, blow nitrogen gas, and stir until it dissolves; control the temperature between 10 and 18°C, slowly add 4.1L of perchloric acid, and control When the temperature is between 10 and 20°C, add 18kg of Beta 101 (i.e., N-bromosuccinimide), and after the addition is completed, keep the temperature at 20°C for 20 minutes, then add 100L of methanol, and stir for 5 minutes; Pull the reaction solution into the existing sodium sulfite solution (dissolve 7-7.36kg of sodium sulfite in 40L of water) and 1280L of water at an internal temperature of 5-10°C in the bromohydrin water analysis tank for water analysis, and the water analysis temperature is controlled ...

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Abstract

The invention belongs to the field of steroid hormone drug synthesis, and particularly relates to a synthesis method of a betamethasone epoxy hydrolyzate, which comprises the following step: by using a betamethasone suppressor as a raw material, carrying out bromohydroxylation reaction and epoxy hydrolysis reaction to obtain the betamethasone epoxy hydrolyzate finished product, thereby enhancing the overall yield of the betamethasone epoxy hydrolyzate by reducing the elutriation running. The method reduces the hydrolysis of the bromohydroxy substance in the reaction, and integrates the steps of epoxidation and hydrolysis into one step, thereby enhancing the yield of the betamethasone epoxy hydrolyzate.

Description

technical field [0001] The invention belongs to the field of synthesis of steroid hormone drugs, in particular to a synthesis method of betamethasone epoxy hydrolyzate. Background technique [0002] Betamethasone is an isomer of dexamethasone. It has the same effect as dexamethasone, but its anti-inflammatory effect is stronger than that of dexamethasone and triamcinolone. It is used to treat active rheumatism and rheumatoid arthritis. , lupus erythematosus, severe bronchial asthma, severe dermatitis, acute leukemia, etc., are also used in the comprehensive treatment of certain infections. [0003] Betamethasone epoxy hydrolyzate is an important intermediate for the synthesis of betamethasone and the main raw material for the synthesis of betamethasone. Molecular formula: C 22 h 28 o 5 , Product aliases: DB11; 9β, 11β-epoxy-16β-methylpregna-1,4-diene-17α,21-diol-3,20-dione; Betamethasone epoxy. CAS No.: 981-34-0, molecular structure: [0004] [0005] The current syn...

Claims

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Application Information

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IPC IPC(8): C07J71/00
CPCC07J71/0015
Inventor 张和明
Owner ZHEJIANG XIANJU XIANLE PHARMA
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