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Compound A1, preparation method thereof and application of compound A1 as pranoprofen impurity

A compound and target compound technology, applied in the field of chemical preparation, can solve problems such as the difficulty of pranoprofen, and achieve the effects of high purity, high application value and high quality

Pending Publication Date: 2021-08-06
SHANDONG RUIAN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The research of pranoprofen impurity can be used for the impurity qualitative and quantitative analysis in the preparation of pranoprofen crude drug, thereby can improve the quality standard of pranoprofen, provides important guiding significance for safe drug use; And pranoprofen Fen commercially available impurity is less, periodical impurity is less for the report of the preparation method of this kind of material, has very big difficulty for further improving the quality of pranoprofen

Method used

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  • Compound A1, preparation method thereof and application of compound A1 as pranoprofen impurity
  • Compound A1, preparation method thereof and application of compound A1 as pranoprofen impurity
  • Compound A1, preparation method thereof and application of compound A1 as pranoprofen impurity

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation method of compound A1, the reaction equation is as follows:

[0037]

[0038] The specific steps include:

[0039] (1) 20 mlthf, stirred, stirred, stirred, then add 2.7 g of Compound B, control temperature 10 ° C to 12 ° C, add 1 g of cesium carbonate and 2 g of water, argon gas protection, carbonate solution droplets After the end of the addition, the control room temperature reaction was 12 hours;

[0040] (2) The reaction was added to 1 g of sodium thiosulfate, and the solvent THF was stirred at room temperature to obtain a concentrate C;

[0041] (3) The concentrate C obtained by step (2) was added to 30 mL of dichloromethane, 20 ml of water and 0.5 g of sodium thiosulfate composition, stirred, depressed, and separated from dichloromethane, concentrated at 20 ° C. Dry, get the concentrate D;

[0042] (4) EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc.

[0043] The compound A1 is used as the application of Pralovprofen imp...

Embodiment 2

[0045] The preparation method of compound A1, the reaction equation is as follows:

[0046]

[0047] The specific steps include:

[0048] (1) 20 mlthf, stirred, stirred, stirred, then add 2.5 g of Compound B, control temperature 12 ° C to 16 ° C, add 1 g of sodium hydroxide and 2 g of water, argon gas protection, sodium hydroxide After the solution was added, the control room temperature reaction was 12 hours;

[0049] (2) 1 g of sodium bisulfite was added to the reaction, and the solvent THF was concentrated at room temperature to obtain a concentrate C;

[0050] (3) The concentrate C obtained by step (2) was added to 30 mL of dichloromethane, 20 ml of water and 0.5 g of sodium hydrogen sodium hydrogen-extracted solvent for extraction, stirring, standing, and separated from dichloromethane, concentrated at 20 ° C. Dry, get the concentrate D;

[0051] (4) The concentrate D obtained by step (3) was purified by 1 cm, high at a diameter of 1 cm, and dichloromethane was eluted to ob...

Embodiment 3

[0054] The preparation method of compound A1, the reaction equation is as follows:

[0055]

[0056]

[0057] The specific steps include:

[0058] (1) 20 mlthf, stirred, stirred, stirred, then add 3.0 g of Compound B, control temperature 16 ° C -18 ° C, 1 g of lithium carbonate and 2 g of water formation, argon-protected, lithium carbonate After the end of the addition, the control room temperature reaction was 12 hours;

[0059] (2) 1 g of sodium sodium sulfide was added, and the solvent THF was concentrated at room temperature to obtain a concentrate C;

[0060] (3) The concentrate C obtained by step (2) was added to 30 mL of dichloromethane, 20 ml of water and 0.5 g of sodium sulfide composition, stirred, stirred, standled, and divided into dichloromethane, concentrated to dryness at 20 ° C. Get concentrate D;

[0061] (4) The concentrate D obtained by step (3) was purified by 1 cm, high by 10 cm silica gel column, and dichloromethane was eluted to give 0.70 g of the target...

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Abstract

The invention discloses a compound A1, a preparation method thereof and an application of the compound A1 as a pranoprofen impurity. A compound B reacts with a strong alkali solution in a reaction solvent under the protection of inert gas to obtain the compound A1. The prepared compound A1 is high in purity after being subjected to structure confirmation and HPLC analysis, is applied to quality research of pranoprofen bulk drugs as the pranoprofen impurity, and provides important guiding significance for safe medication.

Description

[0001] Invention [0002] The present invention is belonging to the field of chemical preparation, and more particularly to a compound A1 and a method thereof and a use as a pullovprofen impurity. Background technique [0003] Praloven, CAS: 52549-17-4, chemical name is 2- (5H- [1] benzopyran [2,3-B] pyridine-7-yl) propionic acid, has significant analgesic , Anti-inflammatory, thermal and resistant effect. [0004] Among the existing synthesis routes involved many carbon ion reactions and rearrangements, there are many impurities produced, and the impurity distribution is querrable. The study of Prasloven impurities can be used in the preparation of the preparation of Prasloven. It can improve the quality standards of Praslovprofen, providing important guiding significance for safety medication; The sale of impurities in Fefen City is less reported on the preparation method of this type of material. It is difficult to further improve the quality of Praloven. Inventive content [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/052G01N30/02G01N30/04
CPCC07D491/052G01N30/02G01N30/04G01N2030/027G01N2030/047
Inventor 任霞李家园刘宗银曹慧敏
Owner SHANDONG RUIAN PHARMA CO LTD
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