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Method for pure water phase preparation of rabeprazole sodium

A technology of rabeprazole sodium and rabeprazole sulfide, applied in the field of medicine, can solve the problems of poor selectivity, long reaction steps and time, low reaction yield and the like, and achieves low cost, easy operation and product yield. high purity effect

Inactive Publication Date: 2012-09-19
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The present invention overcomes the low reaction yield, poor selectivity, and long reaction steps and time in the above-mentioned existing technology for producing rabeprazole sodium.

Method used

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  • Method for pure water phase preparation of rabeprazole sodium
  • Method for pure water phase preparation of rabeprazole sodium
  • Method for pure water phase preparation of rabeprazole sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 24.7g 2-hydroxymethyl-3-methyl-4-(3-methoxypropoxy)pyridine hydrochloride, 15.3g phosphorus oxychloride in reactor, stir, and reaction temperature remains on 45~ 55°C, reflux reaction for 0.5h, 24.2g of the product was obtained, the single-step yield was 91%, and the purity was 99% (HPLC);

Embodiment 2

[0033] Add 12.4g 2-hydroxymethyl-3-methyl-4-(3-methoxypropoxy)pyridine hydrochloride, 6.6g thionyl chloride in the reactor, stir, and the reaction temperature remains at 45~ 55°C, reflux reaction for 0.5h, 12g of the product was obtained, the single-step yield was 90%, and the purity was 99% (HPLC);

Embodiment 3

[0035] Add 12.4g 2-hydroxymethyl-3-methyl-4-(3-methoxypropoxy)pyridine hydrochloride, 6.6g thionyl chloride in the reactor, stir, and the reaction temperature remains at 0~ 30°C, reacted for 5 hours, and obtained 10.3 g of the product, with a single-step yield of 78% and a purity of 95% (HPLC);

[0036] The second condensation reaction:

[0037] Example 1

[0038] Add 15g of 2-mercaptobenzimidazole into the reactor, dissolve in aqueous sodium hydroxide solution (a small amount of acetone can also be added), pH=11~13, 0~55°C, stir, take the first step Example 1 The reaction solution was dripped slowly, kept dripping for 90 minutes, continued to react for 90 minutes, and filtered to obtain 34.3 g of the product, with a yield of more than 99%, a total yield of 90%, and a purity of more than 98% (HPLC).

[0039] Example 2

[0040] Add 7.5g of 2-mercaptobenzimidazole into the reactor, dissolve in aqueous sodium hydroxide solution (a small amount of acetone can also be added), pH...

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Abstract

The invention provides a method for pure water phase preparation of rabeprazole sodium and belongs to the technical field of medicines. The method is characterized in that an intermediate, 2-hydroxymethyl-3-methyl-4-(3-methoxyl propoxy) pyridine hydrochloride, of the rabeprazole sodium is adopted as a raw material to be subjected to chlorination reaction, condensation reaction and oxidation reaction, so as to synthesize the rabeprazole sodium through three steps. The method adopts a novel chlorination reaction system and a novel sodium hypochlorite oxidation system, and can achieve a higher chloridization rate and excellently control a sulfur ether intermediate to be oxidized into sulfoxide; the reaction conditions are wild; both the reaction conversion rate and the reaction selectivity are very high; few reaction by-products are produced; the whole process can be carried out under the condition of no solvent; the content of residual solvent is lowered; time-consuming and toilsome vacuum rectification is not needed; the operation is simplified to a great extent; the process flow is short; and suitability for industrial application is achieved.

Description

technical field [0001] The invention relates to a method for preparing rabeprazole sodium in pure water phase, which belongs to the technical field of medicine. Background technique [0002] Rabeprazole Sodium (Rabeprazole Sodium), its chemical name is 2-{[4-(3-methoxypropoxy)3-methylpyridin-2-yl]methylsulfinyl]-1H-benzene Sodium imidazole, the molecular formula is C 18 h 20 N 3 NaO 3 S, the molecular weight is 381.43, and the structural formula is: [0003] [0004] Rabeprazole sodium is the second-generation proton pump inhibitor after omeprazole and lansoprazole. It was developed by Japan's Eisai Company and was first listed in Japan in 1998. Compared with other proton pump inhibitors The therapeutic effect of similar drugs is faster, better, and has fewer side effects. Rabeprazole specifically inhibits gastric parietal cell H + , K + -ATPase system to block the final stage of gastric acid secretion, enhance gastric mucosal fluid secretion and prostaglandin bio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
Inventor 张华廖春桥
Owner DALIAN UNIV OF TECH
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