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Preparation method for bendazac

A technology of benzylic acid and benzoic acid, applied in the field of benzylic acid preparation, can solve the problems of complex process operation, difficult control, low yield and the like, and achieve the effects of high yield, reduced cost and stable quality

Inactive Publication Date: 2018-01-30
合肥远志医药科技开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Bendazic acid, benzyl ether indazole, benzyl indole acid, English name: bendazac, melting point: 161-163°C, relative density: 1.27g / cm3, 508.2°C at 760mmHg, 261.1°C, 3.78E-11mmHg at 25°C, The molecular formula is C16H14N2O3, which is often used as an anti-inflammatory and analgesic agent. The existing preparation method is complex in process operation, difficult to control, low in yield, and high in cost

Method used

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  • Preparation method for bendazac

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Experimental program
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Embodiment 1

[0020] 1. The preparation of intermediate III, the chemical formula of intermediate III is as follows:

[0021]

[0022] Add 10Kg of o-chlorobenzoic acid, 85g of cuprous oxide, 12Kg of anhydrous sodium carbonate, 21Kg of hydrazine hydrate, and 80Kg of toluene into the reactor, heat up to 85°C and stir for 36 hours. After the reaction is complete, add 24Kg of ethanol when the temperature is lowered to 20°C and stir Centrifuge for 0.5h, evaporate the mother liquor to dryness, evaporate the solid and wash it with beating water, and dry at 50°C for 12h to obtain 6.5Kg of white solid intermediate III with a yield of 75.8%. The o-chlorobenzoic acid can be replaced by o-bromobenzoic acid, Any one of o-iodobenzoic acid, the anhydrous sodium carbonate can be replaced by any one of anhydrous potassium carbonate and sodium hydroxide, the equivalent is 1 to 1.5 equivalents of the raw material, and the hydrazine hydrate can be replaced by hydrochloric acid Hydrazine, the equivalent is 3...

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Abstract

The invention provides a preparation method for bendazac. The preparation method comprises the following steps: adding o-halogen benzoic acid, inorganic alkali, a catalyst, a hydrazine compound and asolvent into a reactor, carrying out stirring at 75 to 110 DEG C for 20 to 48 h, carrying out spin-drying, carrying out extraction with an alcohol extractant, and carrying out washing so as to obtainan intermediate III; successively adding the intermediate III, benzyl chloride, sodium hydroxide and water into the reactor, maintaining the temperature in a range of 20 to 75 DEG C, and carrying outcooling, vacuum filtering and washing so as to obtain an intermediate IV; and successively adding the intermediate IV, potassium hydroxide and glycol dimethyl ether into the reactor, carrying out dissolving and clarification under heating, then dropwise adding a glycol dimethyl ether solution of chloroacetic acid, maintaining the temperature in a range of 60 to 85 DEG C, carrying out stirring for4 h, carrying out spin-drying, adjusting acid until a white solid is extracted, carrying out acid-base purification, and carrying out centrifuging so as to obtain white solid bendazac. The method provided by the invention has the advantages of cheap raw material source, easily controllable process operation, high yield, stable quality, significantly-lowered cost compared with the cost of a conventional method, applicability to industrial production, etc.

Description

technical field [0001] The invention belongs to the field of pharmaceutical preparations, in particular, the invention relates to a preparation method of benzaxacid. Background technique [0002] Bendazic acid, benzyl ether indazole, benzyl indole acid, English name: bendazac, melting point: 161-163°C, relative density: 1.27g / cm3, 508.2°C at 760mmHg, 261.1°C, 3.78E-11mmHg at 25°C, The molecular formula is C16H14N2O3, and it is often used as an anti-inflammatory and analgesic agent. The existing preparation method is complex in process operation, difficult to control, low in yield and high in cost. [0003] The structural formula of Lacosamide is as follows: [0004] Contents of the invention [0005] The invention provides a method for preparing bentaxic acid. The method of the invention has the advantages of cheap source of raw materials, easy control of process operation, high yield, stable quality, significantly lower cost than the existing method, and suitability f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/56
Inventor 邵杨蒋维胡孟奇
Owner 合肥远志医药科技开发有限公司
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