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Method for preparing 2-(4-fluorobenzene formyl) benzamide

A technology of fluorobenzoyl and benzamide, which is applied in the field of preparation of 2-benzamide, can solve the problems of serious environmental pollution, inconvenient use, and high equipment requirements, and achieves low environmental pollution, few by-products, and equipment The effect of less corrosion

Active Publication Date: 2015-04-08
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, SOCl 2 Steam has obvious irritating effect on the respiratory tract and conjunctiva, skin contact with liquid can cause burns, high toxicity, and there are also problems such as relatively expensive, serious environmental pollution, inconvenient use, high requirements for equipment, great damage to equipment, and high production costs. shortcoming

Method used

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  • Method for preparing 2-(4-fluorobenzene formyl) benzamide
  • Method for preparing 2-(4-fluorobenzene formyl) benzamide

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A kind of preparation method of 2-(4-fluorobenzoyl) benzamide, its step is as follows:

[0025] 1) Esterification Add 48.8g of 2-(4-fluorobenzoyl)benzoic acid into 420ml of dichloromethane, stir and dissolve, then add 16g of methanol and 0.016g of concentrated sulfuric acid, and reflux for 4.5h;

[0026] 2) After esterification treatment, add 20% sodium hydroxide aqueous solution to the above-mentioned reaction system, adjust the pH value to 6, distill off the remaining methanol in the reaction, add appropriate amount of water and dichloromethane, and let stand to separate layer, the aqueous phase was extracted 4 times with dichloromethane, the organic phases were combined, and the organic phase was washed with saturated brine until the pH of the washing liquid was 7, then dried with anhydrous magnesium sulfate for one hour, filtered, and the filtrate was evaporated under normal pressure Solvent, after the solvent is evaporated to dryness, 41.16g2-(4-fluorobenzoyl) meth...

Embodiment 2

[0030] A kind of preparation method of 2-(4-fluorobenzoyl) benzamide, its step is as follows:

[0031] 1) Esterification Add 48.8g of 2-(4-fluorobenzoyl)benzoic acid into 420ml of dichloromethane, stir and dissolve, then add 22.4g of methanol and 0.04g of concentrated sulfuric acid, and reflux for 4 hours;

[0032] 2) After esterification treatment, add 20% sodium hydroxide aqueous solution to the above-mentioned reaction system, adjust the pH value to 7, distill off the remaining methanol in the reaction, add appropriate amount of water and dichloromethane, and let stand to separate layer, the aqueous phase was extracted 4 times with dichloromethane, the organic phases were combined, and the organic phase was washed with saturated brine until the pH of the washing liquid was 7, then dried with anhydrous magnesium sulfate for one hour, filtered, and the filtrate was evaporated under normal pressure Solvent, after the solvent is evaporated to dryness, 36.32g2-(4-fluorobenzoyl) ...

Embodiment 3

[0036] A kind of preparation method of 2-(4-fluorobenzoyl) benzamide, its step is as follows:

[0037] 1) Esterification Add 48.8g of 2-(4-fluorobenzoyl)benzoic acid into 420ml of dichloromethane, stir to dissolve, add 19.2g of methanol and 0.06g of concentrated sulfuric acid, and reflux for 4.2h;

[0038] 2) After esterification treatment, add 20% sodium hydroxide aqueous solution to the above-mentioned reaction system, adjust the pH value to 6.5, distill off the remaining methanol in the reaction, add appropriate amount of water and dichloromethane, and let stand to separate layer, the aqueous phase was extracted 4 times with dichloromethane, the organic phases were combined, and the organic phase was washed with saturated brine until the pH of the washing liquid was 7, then dried with anhydrous magnesium sulfate for one hour, filtered, and the filtrate was evaporated under normal pressure Solvent, after the solvent is evaporated to dryness, 38.74g2-(4-fluorobenzoyl) methyl ...

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Abstract

The invention relates to the preparation of fine chemical products, and particularly relates to a method for preparing 2-(4-fluorobenzene formyl) benzamide. The method is implemented by taking a 2-(4-fluorobenzene formyl) benzoic acid as a raw material through carrying out esterification reaction on the 2-(4-fluorobenzene formyl) benzoic acid and methanol firstly, and then carrying out ammonolysis reaction on the obtained product and aqua ammonia. According to the method, thionyl chlorides with large toxicity and irritation are abandoned, and therefore, the method is simple and practical, high in economical efficiency, good in yield, less in side reaction, and less in environmental pollution.

Description

technical field [0001] The invention relates to the preparation of fine chemical products, in particular to a preparation method of 2-(4-fluorobenzoyl)benzamide. Background technique [0002] 2-(4-fluorobenzoyl)benzamide is an important raw material for the synthesis of pitavastatin calcium and other pharmaceutical intermediates. Its English name is 2-(4-Fluorobenzoyl)benzamide, and its molecular formula is C 14 h 10 FNO 2 , the molecular weight is 243.23, the chemical substance registration number is 1548-28-3, the melting point is 177-178°C, and the structural formula is as follows: [0003] [0004] At present, the invention patent application with application number 200410014836.3 discloses a preparation method of 2-(4-fluorobenzoyl)benzamide, which uses 2-(4-fluorobenzoyl)benzoic acid as raw material , with SOCl 2 The acylation reaction is carried out first, and then with NH 3 Prepared by reaction. Among them, SOCl 2 Steam has obvious irritating effect on the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C235/84C07C231/02
Inventor 吴文雷祝冠彬白玉爽徐凤波王文虎李庆山胡方中刘英贤
Owner CHAMBROAD CHEM IND RES INST CO LTD
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