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Preparation method of rupatadine fumarate

A technology for rupatadine fumarate and crude products, which is applied in the field of preparation of rupatadine fumarate, can solve problems such as low yield, low product purity, and harsh reaction conditions, and achieve high yield and high product purity. High and simple preparation process

Inactive Publication Date: 2013-05-15
ANHUI YOUCARE KAIYUE PHARMA
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AI Technical Summary

Problems solved by technology

[0003] The preparation process of rupatadine fumarate in the prior art has many synthetic routes, and there are many defects such as low yield, harsh reaction conditions, and low product purity.

Method used

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Embodiment Construction

[0048] The present invention will be further described below in conjunction with embodiment.

[0049] ①, the preparation of N-(1,1-dimethylethyl)-3-methyl-2-pyridinamide

[0050] In a 2000ml three-necked flask, add 236g (2.0mol) of 3-chloromethyl-5-pyridine hydrochloride and 470ml of tert-butanol, stir, heat up to 60°C, add 240ml of concentrated sulfuric acid dropwise to the reaction mixture, drop Add time is 30 minutes. The temperature of the reaction solution was controlled at 65° C., and the reaction was stirred for 8 hours.

[0051]Lower the temperature of the reaction solution to room temperature, dilute with 240ml of water, add 350ml of toluene, adjust the pH of the solution to 8 with concentrated ammonia water, and separate the organic phase; extract twice with toluene, combine the organic phases, and wash with saturated brine. The organic phase was separated, dried with anhydrous magnesium sulfate, filtered with suction, and the solvent toluene was distilled off unde...

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Abstract

The invention relates to the technical field of pharmaceutical synthesis, and in particular relates to a preparation method of rupatadine fumarate. The preparation method comprises the following steps of: adding 235-237g of 3-chloromethyl-5-pyridine hydrochloride and 465-475ml of tertiary butanol in a reaction container; stirring and heating to 55-65 DEG C; dropping 235-245ml of concentration sulfuric acid, controlling the temperature of the reaction liquid to be 55-65 DEG C and reacting for 8-10 hours; cooling to room temperature, diluting with 234-245ml of water, then adding 345-355ml of methylbenzene, and adjusting pH value of the liquor by stronger ammonia water to 7.8-8.2 to separate out an organic phase; and after water layer extraction, combining the organic phases, washing the organic phase, drying and evaporating to remove the solvent to obtain an oily liquid product. The preparation method of rupatadine fumarate is simple and quick in preparation process, so that the preparation method is suitable for industrialized production. The yield is higher, and the reaction time is effectively shortened. Meanwhile, the refining process is simpler and the product purity is higher.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a preparation method of rupatadine fumarate. Background technique [0002] Rupatadine fumarate is a novel and powerful antiallergic drug developed by Uriach Pharmaceutical Company of Spain, which has dual functions of antihistamine and antagonism of platelet activating factor (PAF). [0003] The preparation process of rupatadine fumarate in the prior art has many synthetic routes, and mostly has defects such as low yield, harsh reaction conditions, and low product purity. Contents of the invention [0004] The present invention aims to overcome the technical problems in the above-mentioned prior art, and proposes a method for preparing rupatadine fumarate with high yield and convenient industrial production. [0005] The technical scheme that the present invention adopts is as follows: [0006] The preparation method of rupatadine fumarate is characterized in that it c...

Claims

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Application Information

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IPC IPC(8): C07D401/14
Inventor 周如国
Owner ANHUI YOUCARE KAIYUE PHARMA
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