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Tetracaine preparation method

A technology of butyl and n-butyraldehyde, which is applied in chemical instruments and methods, cyanide reaction preparation, preparation of organic compounds, etc., can solve the problems of long steps and troublesome operations, and achieves improved yield, reduced pollution, and simplified synthesis. effect of steps

Active Publication Date: 2016-06-08
JINAN CHENGHUI SHUANGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the steps of this method are still long and the operation is cumbersome, so it is necessary to develop a simpler and cleaner synthetic method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0019] Put 50Kg (364.7mol) of p-aminobenzoic acid, 5Kg of 5% palladium carbon and 200Kg of ethanol into the hydrogenation kettle, stir evenly, pass in hydrogen and raise the temperature to 70°C, keep the pressure at 0.1Mpa, add 26.3Kg (364.7mol) of butyraldehyde ), continue hydrogenation for 4 hours after the addition is complete; liquid phase detection of N-butyl p-aminobenzoic acid solution content > 96%, filter to remove palladium carbon for treatment; then transfer the filtered solution to another reaction kettle, stir Add 14.6Kg (364.7mol) of sodium hydroxide, the solution starts to concentrate under reduced pressure until viscous, then add 600Kg of toluene to fractionate to remove ethanol and water, add N,N-dimethylchloroethylamine hydrochloride 53Kg (368mol) and 39Kg (367.9mol) of sodium carbonate was refluxed for 8 hours, then cooled, filtered, the organic layer was washed with water and evaporated to dryness to obtain crude tetracaine. The tetracaine and tetracaine hy...

Embodiment 2

[0021] Put 50Kg (364.7mol) of p-aminobenzoic acid, 5Kg of 5% palladium carbon and 200Kg of ethanol into the hydrogenation kettle, stir evenly, pass in hydrogen and cool down to 10°C, keep the pressure at 0.3Mpa, add 26.3Kg (364.7mol) of butyraldehyde ), hydrogenation was continued for 8 hours after the addition was completed; the content of N-butyl p-aminobenzoic acid solution was detected by liquid phase > 96%, and the palladium carbon was removed by filtration to be treated mechanically; then the filtered solution was transferred to another reaction kettle and stirred Add 14.6Kg (364.7mol) of sodium hydroxide, the solution starts to concentrate under reduced pressure until viscous, then add 600Kg of toluene to fractionate to remove ethanol and water, add N,N-dimethylchloroethylamine hydrochloride 53Kg (368mol) and 39Kg (367.9mol) of sodium carbonate was refluxed for 8 hours, then cooled, filtered, the organic layer was washed with water and evaporated to dryness to obtain cru...

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PUM

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Abstract

The invention discloses a tetracaine preparation method, comprising the following steps in sequence: (1) performing a catalytic reduction reaction on para aminobenzoic acid and n-butanal to prepare N-butyl para aminobenzoic acid; (2) filtering reaction liquid obtained in step (1), then adding sodium hydroxide for mixing; (3) enabling the N-butyl para aminobenzoic acid treated by the sodium hydroxide to directly react with N,N-dimethyl chloroethylamine hydrochloride without refining and separation, thus obtaining tetracaine. According to the method, the steps are fewer, the operation is simple, more convenience and cleanness are realized, and the product yield is higher.

Description

technical field [0001] The invention relates to a preparation method of a local anesthetic, in particular to a method for preparing tetracaine. Background technique [0002] Tetracaine and tetracaine hydrochloride are commonly used local anesthetics in clinic. The disclosed preparation method uses benzocaine as a raw material for synthesis, and the steps are relatively long and the pollution is large. The method disclosed in CN102731333 uses p-aminobenzoic acid as the starting material, forms a Schiff base with butyraldehyde and then undergoes catalytic hydrogenation under alkaline conditions to obtain N-butyl p-aminobenzoic acid, and then crystallizes in the presence of sulfuric acid React with N,N-dimethylethanolamine to get tetracaine. [0003] However, the steps of this method are still long and the operation is cumbersome, so it is necessary to develop a simpler and cleaner synthesis method. Contents of the invention [0004] The object of the present invention is ...

Claims

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Application Information

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IPC IPC(8): C07C229/60C07C227/18
CPCC07C227/18C07C229/60
Inventor 刘浩王寅孟德勇赵会清李跃东
Owner JINAN CHENGHUI SHUANGDA CHEM
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