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Synthesis 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, simple operation and convenient operation

Active Publication Date: 2019-08-02
BIONNA (BEIJING) MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Synthesis method of budesonide impurity USP-Z1
  • Synthesis method of budesonide impurity USP-Z1
  • Synthesis method of budesonide impurity USP-Z1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0024]

[0025] Take 8.6g of budesonide in a 250mL three-neck bottle, add 80mL of 1,4-dioxane to dissolve, cool down to 0-10°C, add 6.06g of triethylamine as an acid-binding agent and 5.32g of butyryl chloride, control The temperature is not higher than 20°C, keep warm for 1-2 hours; after the reaction is completed, place the obtained reaction solution in 100mL water to quench the reaction, add 100mL dichloromethane for extraction, collect the organic phase and continue to dilute the water phase with 100mL dichloromethane Secondary extraction with methyl chloride, combining the organic phases obtained twice, successively using 50mL saturated sodium chloride solution and 50mL water to wash the organic phase, and evaporating the organic solvent under reduced pressure to obtain a foamy solid; adding 50mL of dichloromethane to the resulting foamy solid Dissolve, add petroleum ether at room temperature until cloudy, stop, crystal...

Embodiment 2

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

[0031]

[0032] Take 3.9g of budesonide in a 100mL three-necked bottle, add 40mL of 1,4-dioxane to dissolve, cool down to 0-10°C, add 2.94g of triethylamine as an acid-binding agent and 2.47g of butyric anhydride, control The temperature is not higher than 20°C, keep warm for 1-2 hours; after the reaction is completed, put the obtained reaction solution in 50mL water to quench the reaction, add 50mL dichloromethane to extract, collect the organic phase and continue to dilute the water phase with 50mL dichloromethane Chloromethane secondary extraction, combined two organic phases obtained, successively adopt 24mL saturated sodium chloride solution and 24mL water to wash the organic phase, evaporate the organic solvent under reduced pressure to obtain a foamy solid; add 25mL dichloromethane to the obtained foamy solid Dissolve, add petroleum ether at room temperature until cloudy, stop, crystallize at room temperature for 2 ho...

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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, in particular to a method for synthesizing budesonide impurity USP-Z1. Background technique [0002] Budesonide is a glucocorticoid asthma treatment drug, which belongs to the adrenal cortex hormone drugs. It was first developed and marketed by AstraZeneca Pharmaceutical Company in 1981. It has a strong local anti-inflammatory effect, can inhibit early bronchospasm and late allergic reaction, and is one of the important drugs for the treatment of allergic asthma. Among similar drugs, budesonide has highly effective local anti-inflammatory effect, long-lasting effect and no systemic adrenal cortex hormone effect, so it is more suitable for local administration. [0003] At present, budesonide is mainly used in the treatment of asthma and allergic rhinitis in two different dosage forms, aerosol and suspension respectively. The dosage forms with budesonide as the active ingredient on the mar...

Claims

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Application Information

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Patent Type & Authority Applications(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
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