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Method for detecting contents of dolasetron isomer and salt thereof

A technology of dolasetron and detection method is applied in the field of determination of drug content, and can solve the problems of preparation, confirmation, biological activity and detection method of dolasetron isomers that have not been seen

Active Publication Date: 2013-04-24
LIAONING HAISCO PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there are no research reports on the preparation, confirmation, biological activity and detection methods of dolasetron isomers

Method used

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  • Method for detecting contents of dolasetron isomer and salt thereof
  • Method for detecting contents of dolasetron isomer and salt thereof
  • Method for detecting contents of dolasetron isomer and salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] Example 1 Preparation of cis-7-ethoxycarbonyl-9-(ethoxycarbonylmethyl)-9-azabicyclo-[3,3,1]nonan-3-ol

[0088] Put 100g of 7-ethoxycarbonyl-9-(ethoxycarbonylmethyl)-9-azabicyclo-[3,3,1]non-3-one, 500ml of tetrahydrofuran and 10g of Raney nickel into the autoclave , feed hydrogen to a pressure of 0.1Mpa; slowly heat up to 90-100°C, adjust the hydrogen pressure to 0.5-0.6Mpa, stir until the reaction is complete, cool to room temperature, and filter the reaction solution through diatomaceous earth to remove Raney nickel , after the obtained filtrate was concentrated and dried under reduced pressure, the obtained brown-yellow oil was purified through a silica gel column (980 g of 200-300 mesh silica gel, packed with petroleum ether, washed with ethyl acetate / petroleum ether (1 / 10-1 / 5) deagent), to obtain light yellow oil 12g.

Embodiment 2

[0089] Example 2 Preparation of cis-7-ethoxycarbonyl-9-(ethoxycarbonylmethyl)-9-azabicyclo-[3,3,1]nonan-3-ol

[0090] Dissolve 100g of 7-ethoxycarbonyl-9-(ethoxycarbonylmethyl)-9-azabicyclo-[3,3,1]nonan-3-one with 500ml of absolute ethanol and add 12.5g in batches Sodium borohydride, heating to reflux, stirring, until the reaction is complete, add concentrated hydrochloric acid dropwise, adjust the pH of the reaction solution to 7~8, recover ethanol under reduced pressure, add water to dissolve the obtained concentrate after cooling, and extract to the water phase with ethyl acetate There was no product, the ethyl acetate layers were combined and dried with anhydrous sodium sulfate, anhydrous sodium sulfate was filtered off, the filtrate was concentrated to dryness under reduced pressure, and the obtained concentrate was purified on a silica gel column (950 g of 200-300 mesh silica gel, packed in petroleum ether, washed The deagent is ethyl acetate / petroleum ether (1 / 10~1 / 5)...

Embodiment 3

[0091] Example 3 Preparation of cis-7-ethoxycarbonyl-9-(ethoxycarbonylmethyl)-9-azabicyclo[3,3,1]nonan-3-ol-2-tetrahydropyranyl ether

[0092] Dissolve 20 g of cis-7-ethoxycarbonyl-9-(ethoxycarbonylmethyl)-9-azabicyclo-[3,3,1]nonan-3-ol in 100 ml of dichloromethane, cool in an ice bath, Slowly add 6g of methanesulfonic acid dropwise, then add 6g of 3,4-dihydropyran dropwise, stir until the reaction is complete, transfer the reaction solution into 200g of 40% potassium carbonate solution, extract with ethyl acetate, take the ethyl acetate layer It was dried with anhydrous sodium sulfate, filtered to remove anhydrous sodium sulfate, and the filtrate was concentrated to dryness under reduced pressure to obtain 24 g of brown-yellow oil.

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Abstract

The invention relates to a method for detecting the contents of dolasetron or isomers in dolasetron salt or dolasetron salt by adopting high performance liquid chromatography. According to the method, normal phase chromatography hu or reversed phase chromatography is adopted to determine the content of isomers of dolasetron or dolasetron salt raw material or preparations (such as oral preparations and injections). The detection method of the invention can better separate dolasetron from isomers, and excellently detects and controls the content of isomers of dolasetron or dolasetron salt raw material or dolasetron preparations (such as oral preparations and injections) to guarantee safety effectiveness of drugs.

Description

technical field [0001] The invention belongs to the field of determination of drug content, in particular to a detection method for the content of dolasetron isomers and salts thereof. Background technique [0002] In recent years, the market sales of antiemetic drugs have been increasing year by year, and their market share in digestive system drugs ranks second only to antiulcer drugs. [0003] Dolasetron and its salts are potent and highly selective 5-HT 3 Receptor antagonists are clinically used to prevent and treat nausea and vomiting in tumor patients during chemotherapy and after gynecological operations and surgical operations, with mild adverse reactions. Specifically, the clinical therapeutic applications of dolasetron and its salts mainly include: 1) prevention of nausea and vomiting associated with naïve and re-treated emetogenic tumor chemotherapy (including high-dose cisplatin), strongly inhibiting cisplatin, adriamycin 2) Prevention of postoperative nausea a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/89G01N30/60C07D471/18C07D451/14
Inventor 邹欣王晓玲谢成莲蒲洪许娟韩娟
Owner LIAONING HAISCO PHARMACEUTICAL CO LTD
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