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A kind of synthetic method of budesonide impurity usp-z1

A USP-Z1, USP-Z1-IM1 technology, applied in the field of drug impurity synthesis, to achieve the effect of simple process route, convenient operation and high yield

Active Publication Date: 2020-04-28
BIONNA (BEIJING) MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, there is no synthetic method specifically for budesonide impurity USP-Z1 in the prior art

Method used

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  • A kind of synthetic method of budesonide impurity usp-z1
  • A kind of synthetic method of budesonide impurity usp-z1
  • A kind of synthetic method of budesonide impurity usp-z1

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step 1: Synthesis of compound USP-Z1-IM1

[0024]

[0025] Take 8.6g budesonide in a 250mL three-necked flask, add 80mL 1,4-dioxane to dissolve, cool to 0~10℃, add 6.06g triethylamine as acid binding agent and 5.32g butyryl chloride, control The temperature is not higher than 20℃, and the reaction is kept for 1~2h; after the reaction is completed, the obtained reaction solution is placed in 100 mL of water for quenching reaction, 100 mL of dichloromethane is added for extraction, the organic phase is collected and the water phase is continued with 100 mL of water. Extract the organic phase twice with methyl chloride, combine the organic phases obtained twice, wash the organic phase with 50 mL saturated sodium chloride solution and 50 mL water, and evaporate the organic solvent under reduced pressure to obtain a foam solid; add 50 mL dichloromethane to the obtained foam solid After dissolving, adding petroleum ether at room temperature until turbidity stopped, crystallizing...

Embodiment 2

[0030] Step 1: Synthesis of compound USP-Z1-IM1

[0031]

[0032] Take 3.9g budesonide in a 100mL three-necked flask, add 40mL 1,4-dioxane to dissolve, cool to 0~10℃, add 2.94g triethylamine as acid binding agent and 2.47g butyric anhydride, control The temperature is not higher than 20℃, and the reaction is kept for 1~2h; after the reaction is completed, the obtained reaction solution is placed in 50mL water for quenching reaction, 50mL dichloromethane is added for extraction, the organic phase is collected and the water phase is continued to The organic phase was extracted twice with methyl chloride, and the organic phases obtained twice were combined. The organic phase was washed successively with 24 mL of saturated sodium chloride solution and 24 mL of water, and the organic solvent was evaporated under reduced pressure to obtain a foamed solid; 25 mL of dichloromethane was added to the obtained foamed solid Dissolve, add petroleum ether at room temperature to stop when it be...

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Abstract

The invention provides a synthesis method of a budesonide impurity USP-Z1. According to the synthesis method, firstly, budesonide is taken as a raw material and subjected to a reaction with butyryl chloride or butyric anhydride under the condition of an organic solvent and an acid-binding agent to produce a compound USP-Z1-IM1; then, the compound USP-Z1-IM1 is dissolved in the organic solvent, anoxidant is added, oxidation is performed, and the impurity USP-Z1 is produced. The synthesis method adopts a simple process route and is convenient to operate, good in selectivity and high in yield; the synthesized budesonide impurity USP-Z1 can serve as a reference substance for detection and study of budesonide and is applied to quality control of budesonide and related preparations to control the purity of raw materials or preparations of budesonide.

Description

Technical field [0001] The invention belongs to the field of drug impurity synthesis, and particularly relates to a method for synthesizing budesonide impurity USP-Z1. Background technique [0002] Budesonide is a kind of glucocorticoid asthma treatment medicine, which belongs to adrenocorticoid medicine. It was first developed and marketed by AstraZeneca Pharmaceuticals in 1981. It has a strong local anti-inflammatory effect and can inhibit early bronchospasm and late allergic reactions. It is one of the important drugs for the treatment of allergic asthma. Among similar drugs, budesonide has a highly effective local anti-inflammatory effect, with a long acting time and no systemic adrenal cortex hormone effect. It is more suitable for topical medication. [0003] At present, budesonide is mainly used for the treatment of asthma and allergic rhinitis in two different dosage forms: aerosol and suspension. The dosage forms with budesonide as the active ingredient on the market in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
CPCC07J71/0031
Inventor 李久青蔡报彬浮绍东李昊蔡保理
Owner BIONNA (BEIJING) MEDICAL TECH CO LTD