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Preparation method of p-methoxyphenylethylamine

A technology of methoxyphenethylamine and methoxyphenylpropanamide, which is applied in the field of preparation of p-methoxyphenethylamine, can solve the problems of environmental pollution and low yield, achieve high yield, simple process, The effect of mild reaction conditions

Active Publication Date: 2020-08-11
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the defects of environmental pollution and low yield in the preparation of p-methoxyphenylethylamine in the prior art, the present invention provides a green, environmentally friendly and efficient preparation method of p-methoxyphenylethylamine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method for p-methoxyphenethylamine, comprising the steps of:

[0022] (1) Dissolve 0.55 mol of sodium hydroxide in 150 mL of water to obtain a sodium hydroxide alkali solution, add 0.0135 mol of sodium bromide to the sodium hydroxide alkali solution, stir well, then add 0.28 mol of p-methoxyphenylpropane Amide, mixed uniformly to obtain the first solution;

[0023] (2) heating described first solution to 50 ℃, dripping concentration under stirring condition is 28wt% hydrogen peroxide (H 2 o 2 The number of moles is 0.28mol), the temperature is raised to 60° C., and the Hoffman reaction is carried out for 30 minutes;

[0024] (3) Cool the reaction solution after step (2) to 15° C., extract with dichloromethane, and remove the solvent to obtain 41.2 g of light yellow oily p-methoxyphenethylamine, the content is 98.9%, and the yield was 96.3%.

Embodiment 2

[0026] A preparation method for p-methoxyphenethylamine, comprising the steps of:

[0027] (1) Dissolve 0.60 mol of sodium hydroxide in 120 mL of water to obtain a sodium hydroxide alkaline solution, add 0.0155 mol of sodium bromide to the sodium hydroxide alkaline solution, stir well, then add 0.28 mol of p-methoxyphenylpropane Amide, mixed uniformly to obtain the first solution;

[0028] (2) heating described first solution to 56 ℃, dripping concentration under stirring condition is 28wt% hydrogen peroxide (H 2 o 2 The number of moles is 0.28mol), the temperature was raised to 64°C, and the Hoffman reaction was carried out for 40min;

[0029] (3) Cool the reaction solution after the reaction in step (2) to 20° C., extract with dichloromethane, and remove the solvent to obtain 41.6 g of p-methoxyphenethylamine in light yellow oil, with a content of 99.0%, and a yield of was 97.3%.

Embodiment 3

[0031] A preparation method for p-methoxyphenethylamine, comprising the steps of:

[0032] (1) Dissolve 0.50 mol of sodium hydroxide in 150 mL of water to obtain a sodium hydroxide alkaline solution, add 0.0150 mol of sodium bromide to the sodium hydroxide alkaline solution, stir well, then add 0.28 mol of p-methoxyphenylpropane Amide, mixed uniformly to obtain the first solution;

[0033] (2) heating described first solution to 56 ℃, dripping concentration under stirring condition is 28wt% hydrogen peroxide (H 2 o 2 The number of moles is 0.28mol), the temperature was raised to 62°C, and the Hoffman reaction was carried out for 45min;

[0034] (3) Cool the reaction solution after step (2) to 20° C., extract with dichloromethane, and remove the solvent to obtain 42.1 g of light yellow oily p-methoxyphenethylamine, the content is 98.0%, and the yield was 97.4%.

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method of p-methoxyphenylethylamine, which comprises: (1) adding sodium bromide to an alkali solution, uniformly stirring, adding p-methoxybenzamide, and uniformly mixing to obtain a first solution; (2) heating the first solution, dropwise adding hydrogen peroxide with the concentration of 28wt% under a stirring condition, heating, reacting the hydrogen peroxide with sodium bromide to generate sodium hypobromite, and further carrying out a Hofmann reaction on the sodium hypobromite and amide; and (3) cooling, extracting and desolventizing the reaction solution after the reaction in the step (2) to obtain light yellow oily p-methoxyphenylethylamine. The preparation method has the beneficial effects that the green reagent hydrogen peroxide is used for replacing sodium hypochlorite (or sodium hypobromite), the alkali consumption can be reduced, the salt content of a reaction system is greatly reduced, the reaction conditions are mild and controllable, the yield is high, the cost is low, and the preparation method is suitable for industrial production and use.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of p-methoxyphenethylamine. Background technique [0002] P-methoxyphenethylamine is an important intermediate in organic synthesis and pharmaceutical industry. The development and research of p-methoxyphenethylamine has attracted the attention of chemical researchers. In the prior art, most p-methoxyphenylethylamine adopts chlorine gas or sodium hypochlorite as oxidizing agent, utilizes Hoffmann reaction that p-methoxyphenylpropanamide is oxidized to obtain p-methoxyphenylethylamine, but chlorine (very toxic ) or sodium hypobromite (chlorine) (high salt content) is more complicated as the process of oxidant, and the risk factor is higher, which is not friendly to the environment. [0003] Therefore, how to provide a kind of green pollution-free, the method for preparing p-methoxyphenethylamine with high yield seems particularly important. Con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C213/10C07C217/60
CPCC07C213/02C07C213/10C07C217/60
Inventor 郭建国秦建国吴孝兰夏晓晗
Owner SINOPHARM CHEM REAGENT