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A kind of environment-friendly preparation method of ibuprofen impurity h

A technology for impurities and compounds, which is applied in the field of preparation of pharmaceutical impurity standards to achieve the effects of less by-products, high purity and easy purification

Active Publication Date: 2021-01-19
深圳市祥根生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report about the preparation method of ibuprofen impurity H, especially the preparation method of high-purity ibuprofen impurity H

Method used

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  • A kind of environment-friendly preparation method of ibuprofen impurity h
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  • A kind of environment-friendly preparation method of ibuprofen impurity h

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preparation example Construction

[0032] The preparation method provided by this implementation method has the advantages of simple operation, short preparation cycle, few by-products, easy purification, high yield, and environmental protection. The yield of the profen impurity H is at least 35.00%, and the prepared ibuprofen impurity H The purity of the product is at least 99.00%, without obvious impurity points, and meets the requirements of the impurity reference substance. It can be used as the standard substance of ibuprofen impurity H, and can be used in the qualitative and quantitative research and detection of ibuprofen impurity H. For ibuprofen and its related The quality control of preparations has certain significance.

[0033] One embodiment of the present invention also provides a method for detecting the impurity H of ibuprofen, the standard substance used is the impurity H of ibuprofen mentioned above. The above-mentioned ibuprofen impurity H has relatively high purity, which can improve the acc...

Embodiment 1

[0041] A kind of environmental protection preparation method of ibuprofen impurity H, comprises the following steps:

[0042] Step 1: Mix 0.5g of the compound shown in formula (I) with 0.543g of the compound shown in formula (II) and dissolve in EtOH, then dissolve 0.42g of NaOC at 60-80°C 2 h 5 Add to it in 4 batches, stir the reaction for 12h, remove the EtOH by rotary evaporation of the reaction solution, then dissolve the obtained solid, separate and purify by column chromatography, the eluent is PE:EA=10:1, and the formula (III ) compound;

[0043] Step 2: Dissolve 0.5 g of the compound represented by formula (III) in anhydrous THF, and slowly add 1.56 mL of CH with a concentration of 1 mol / L at -20°C 3 MgBr reagent, compound shown in formula (III) and CH 3 The molar ratio of MgBr is 1:1, stirred and reacted at this temperature for 60min, the reaction solution was rotary evaporated to remove THF, and separated and purified by column chromatography, the eluent was PE:EA...

Embodiment 2

[0056] A kind of environmental protection preparation method of ibuprofen impurity H, comprises the following steps:

[0057] Step 1: 0.5g of the compound shown in formula (I) and 0.543g of the compound shown in formula (II) were mixed and dissolved in EtOH, and then 0.315g of NaOC was dissolved at 60-80°C 2 h 5 Add to it in 4 batches, stir the reaction for 15h, remove the EtOH by rotary evaporation of the reaction liquid, then dissolve the obtained solid, separate and purify by column chromatography, the eluent is PE:EA=8:1, and the formula (III ) compound;

[0058] Step 2: Dissolve 0.5 g of the compound represented by formula (III) in anhydrous THF, and slowly add 1.56 mL of CH with a concentration of 1 mol / L at -20°C 3 MgBr reagent, compound shown in formula (III) and CH 3 The molar ratio of MgBr is 1:1, stirred and reacted at this temperature for 60min, the reaction solution was rotary evaporated to remove THF, and separated and purified by column chromatography, the el...

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Abstract

The invention provides an environment-friendly preparation method of an ibuprofen impurity H, and belongs to the technical field of preparation of drug impurity standard substances. The method comprises the following steps: step 1, reacting a compound shown as a formula (I) with a compound shown as a formula (II) under the catalytic action of NaOC2H5 to prepare a compound shown as a formula (III);and step 2, reacting the compound shown in the formula (III) in the presence of CH3MgBr to prepare the ibuprofen impurity H. The method has the advantages of simplicity in operation, short preparation period, few byproducts, easiness in purification, high yield and environmental friendliness; the prepared ibuprofen impurity H is high in purity and free of obvious impurity points and meets the requirements of impurity reference substances and can be used as an ibuprofen impurity H standard substance to be applied to qualitative and quantitative research and detection of the ibuprofen impurityH so as to improve the accuracy of the detection method.

Description

technical field [0001] The invention belongs to the technical field of preparation of drug impurity standard products, and in particular relates to an environment-friendly preparation method of ibuprofen impurity H. Background technique [0002] Ibuprofen (Ibuprofen), the chemical name is 2-(4-isobutylphenyl)propionic acid, and its Chinese alias is Ba Nufeng. It is a non-steroidal anti-inflammatory drug widely used clinically, belonging to aryl alkanoic drugs. Ibuprofen can be used as a substitute for aspirin, and has stronger antipyretic, anti-inflammatory and analgesic effects. It is mainly used for the control of inflammation and pain in diseases such as colds, rheumatism and rheumatoid arthritis, while the side effects are much smaller than aspirin . European Pharmacopoeia, British Pharmacopoeia, American Pharmacopoeia, Pharmacopoeia, and Chinese Pharmacopoeia all record the variety of ibuprofen, and the determination of its related substances is also described in deta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/69C07C49/782C07C45/74C07C49/796G01N30/02
CPCC07C45/69C07C45/74C07C49/782G01N30/02C07C49/796
Inventor 李方林
Owner 深圳市祥根生物科技有限公司
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