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A kind of method for preparing tetracaine

A technology of butyl and n-butyraldehyde, applied in chemical instruments and methods, preparation of cyanide reaction, preparation of organic compounds, etc., can solve problems such as long steps and troublesome operation, and achieve increased yield, reduced pollution, and simplified synthesis The effect of steps

Active Publication Date: 2018-02-16
JINAN CHENGHUI SHUANGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

[0018] 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

[0020] 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 method for preparing tetracaine, which comprises the following steps in sequence: (1) preparing N-butyl p-aminobenzoic acid through catalytic reduction reaction of p-aminobenzoic acid and n-butyraldehyde; (2) in step (1) (3) N-butyl p-aminobenzoic acid treated with sodium hydroxide is directly reacted with N,N-dimethylchloroethylamine hydrochloride without purification and separation Tetracaine. The method of the invention has few steps, simple operation, easier cleaning and higher product yield.

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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Patent Type & Authority Patents(China)
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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