Preparation method for sarpogrelate hydrochloride photodegradable impurity III

A technology of sarcogrelate hydrochloride and photodegradation, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of aminohydroxyl compounds, etc., can solve the problems of lack of literature and patent reports, etc.

Inactive Publication Date: 2016-01-13
SHANDONG QIDU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are no literature and patent reports on the preparation method of sagrelate hydrochloride photodegradation impurities. In order to better carry out quality research on sarcogrelate hydrochloride raw materials and ensure product quality, the inventors have carried out photodegradation of sarcogrelate hydrochloride. The chemical synthesis of impurities was studied, and a preparation method of high-purity photodegradation impurities was obtained, which provided a guarantee for improving the quality of sargrel hydrochloride raw materials

Method used

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  • Preparation method for sarpogrelate hydrochloride photodegradable impurity III
  • Preparation method for sarpogrelate hydrochloride photodegradable impurity III
  • Preparation method for sarpogrelate hydrochloride photodegradable impurity III

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] Salicylaldehyde (10.0g, 82mmol) was added to a 250ml reaction flask, 100ml of tetrahydrofuran was added, epichlorohydrin (9.1g, 98mmol) and 10g of potassium carbonate were added, under nitrogen protection, the temperature was raised to reflux, and reacted for 12h. TLC detects that the raw material has been reacted (petroleum ether: ethyl acetate=4:1v / v), and the product 2-(2-oxomethyloxirane) benzaldehyde II-2 is obtained after post-treatment, post-treatment: suction filtration Potassium carbonate was removed, and the filtrate was concentrated by distillation under reduced pressure to obtain compound 2-(2-oxomethyloxirane)benzaldehyde II-2, 10.39 g, yield 71.2%.

Embodiment 2

[0094] Salicylaldehyde (10.0g, 82mmol) was added to a 250ml reaction flask, 100ml of tetrahydrofuran was added, epichlorohydrin (9.1g, 98mmol) and 5g of potassium hydroxide were added, under nitrogen protection, the temperature was raised to reflux, and reacted for 15h. TLC detects that the raw material has been reacted (petroleum ether: ethyl acetate=4:1v / v), and the product 2-(2-oxomethyloxirane) benzaldehyde II-2 is obtained after post-treatment, post-treatment: suction filtration Potassium carbonate was removed, and the filtrate was concentrated by distillation under reduced pressure to obtain compound 2-(2-oxomethyloxirane)benzaldehyde II-2, 8.76 g, yield 60.0%.

Embodiment 3

[0096] Compound 2-(2-oxomethyloxirane)benzaldehyde (10.0g, 60mmol) was dissolved in 100ml of tetrahydrofuran, cooled to 0°C, added 10g of 40% dimethylamine aqueous solution, and reacted at room temperature for 4h, TLC Tracking (petroleum ether: ethyl acetate = 4:1 v / v). Concentrate after completion of the reaction, extract with ethyl acetate (100*3ml), dry the organic phase over anhydrous sodium sulfate, and concentrate to obtain 2-[2-(dimethylamino)-1-hydroxyethoxy]benzaldehyde II- 3, 11.22 g, yield 89.6%.

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Abstract

The invention belongs to the field of synthesis of medicines, and specifically relates to a preparation method for a sarpogrelate hydrochloride photodegradable impurity III. The sarpogrelate hydrochloride photodegradable impurity III is prepared by comprising five-step reactions of substitution reaction, addition reaction, esterification reaction, epoxidation reaction and reduction reaction with 2-[2-(3-methoxyphenyl)vinyl]phenol as a raw material; and after column chromatography separation of a crude sarpogrelate hydrochloride photodegradable impurity III, purity reaches more than 99%. The preparation method provided by the invention has simple operation and mild reaction; the sarpogrelate hydrochloride photodegradable impurity III has high purity and can be applied in analysis of impurity profiling; and total yield is high.

Description

[0001] This application is a divisional application with application number 201410491531.5, application date September 23, 2014, and invention name "Preparation Method for Photodegradation of Impurities with Sagrelate Hydrochloride". technical field [0002] The invention belongs to the field of drug synthesis, and in particular relates to a preparation method for photodegradation of impurity III by sargrelate hydrochloride. Background technique [0003] Sagrelate Hydrochloride Tablets was first launched in Japan in 1993 under the trade name Anplag, which is a 5-HT2 receptor blocker that can inhibit platelet aggregation and vasoconstriction, has antithrombotic effect and improves microcirculation. Its indications are to improve ischemic symptoms such as ulcers, pain and cold sensation caused by chronic arterial occlusive disease. The sarcogrelate hydrochloride raw material drug used for the preparation of sarcogrelate hydrochloride tablets needs to meet the required purity, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C213/08C07C219/08
Inventor 孔令金李宗涛张涛董旭
Owner SHANDONG QIDU PHARMA
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