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Industrial production method of isothipendyl technical material

A kind of technology of azipromazine and production method, which is applied in the field of production technology of the former drug of azipromazine, can solve the problems such as no production technology report, and achieves the effect of less equipment investment and simple technology

Inactive Publication Date: 2013-02-13
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no relevant production process reports at home and abroad

Method used

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  • Industrial production method of isothipendyl technical material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Under the protection of nitrogen, 100kg of anhydrous acetonitrile was poured into a 300L reaction kettle through a metering pump from an acetonitrile storage tank, and 20kg of 1-azaphenothiazine and 2.4kg of sodium hydride were added through the feeding port. Material at 30 o After C reacted for 1 hour, open the steam valve, pass steam into the jacket of the reaction kettle, and reflux for 2 hours; 3h. When the material is cooled to 30 o C. Filter out the insoluble matter through the filtration system, and then return the acetonitrile mother liquor to the reaction kettle from the storage tank. Hydrogen chloride is blown into the above-mentioned acetonitrile mother liquor through a vaporizer, a buffer tank, and a flow meter, and white crystals are precipitated in the system. HPLC traces that the azipromazine in the mother liquor disappears, and the reaction is stopped. The above-mentioned materials were separated by centrifugation, washed with frozen ethanol, centrifu...

Embodiment 2

[0020] Under the protection of nitrogen, 140kg of anhydrous acetonitrile was poured into the 300L reaction kettle through the metering pump from the acetonitrile storage tank, and 20kg of 1-azaphenothiazine and 2.5kg of sodium hydride were added through the feeding port. Material at 30 o After C reacted for 1 hour, open the steam valve, pass steam into the jacket of the reaction kettle, and reflux for 2 hours; 3h. When the material is cooled to 30 o C. Filter out the insoluble matter through the filtration system, and then return the acetonitrile mother liquor to the reaction kettle from the storage tank. Hydrogen chloride is blown into the above-mentioned acetonitrile mother liquor through a vaporizer, a buffer tank, and a flow meter, and white crystals are precipitated in the system. HPLC traces that the azipromazine in the mother liquor disappears, and the reaction is stopped. The above materials were centrifuged, washed with frozen ethanol, centrifuged again, and dried ...

Embodiment 3

[0023] Under the protection of nitrogen, 200kg of anhydrous acetonitrile was poured into the 300L reaction kettle through the metering pump from the acetonitrile storage tank, and 20kg of 1-azaphenothiazine and 2.7kg of sodium hydride were added through the feeding port. Material at 30 o After C reaction for 1 hour, open the steam valve, pass steam into the jacket of the reaction kettle, and reflux for 2 hours; then add 31.3 kg of 1-p-toluenesulfonyl-2-N,N-dimethylpropylamine through the feeding port, and reflux reaction 3h. When the material is cooled to 30 o C. Filter out the insoluble matter through the filtration system, and then return the acetonitrile mother liquor to the reaction kettle from the storage tank. Hydrogen chloride is blown into the above-mentioned acetonitrile mother liquor through a vaporizer, a buffer tank, and a flow meter, and white crystals are precipitated in the system. HPLC traces that the azipromazine in the mother liquor disappears, and the reac...

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Abstract

The invention provides an industrial production method of an isothipendyl technical material, and belongs to the technical field of anti-anaphylaxis medicines. The preparation method is carried out according to the following steps: feeding 1-azaphenothiazine, sodium hydride and anhydrous acetonitrile in a reaction kettle according to a certain ratio under the protection of nitrogen, reacting for 1h at 30 DEG C, opening a steam valve, introducing steam in a jacket of the reaction kettle, reflowing and reacting for 2h; feeding 1-para-toluene sulfonyl-2-N and N-dimethyl propylamine according to a certain ratio, keeping on reflowing and reacting for 3h, cooling reaction mass to be normal temperature, filtering un-dissolved material away, pumping dry hydrogen chloride in collected acetonitrile solution to obtain isothipendyl hydrochloride white crystals, refining, and finally obtaining the isothipendyl, wherein the purity is higher than 99% and the yield is higher than 70%. According to the invention, the continuous reaction is used, an intermediate product does not need to be separated; the preparation method has the following advantages of simple process, low equipment investment, and the like; the purity of the produced isothipendyl is over 99% and the yield is over 70%, so that the preparation method is beneficial for industrial production.

Description

technical field [0001] The invention belongs to the technical field of antiallergic drugs, and in particular relates to a production process of the original drug of azipromazine. Background technique [0002] Azipromazine belongs to a new type of antihistamine in antiallergic drugs, which belongs to H1 receptor antagonist, and its structural formula is: [0003] [0004] Azipromazine is mainly used to treat diseases such as urticaria, asthma, allergic rhinitis, allergic dermatitis, itchy skin, and colds, and is also effective for skin burns and scalds. Azopromethazine is used as a sunscreen in sunscreen oils because of its photobiochemical properties and can block UVB rays. At present, there are no related production process reports at home and abroad. [0005] Contents of the invention [0006] The object of the present invention is to provide a kind of production method of azipromazine with simple technique and high yield. [0007] The present invention adopts fol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D513/04
Inventor 方永勤褚俊轩武安邦许亮
Owner CHANGZHOU UNIV