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Microwave-assisted rapid synthesis method of N-1-naphthyl ethylenediamine hydrochloride

A naphthyl ethylenediamine hydrochloride, microwave-assisted technology, applied in the field of preparation and purification of organic compounds, can solve the problems of ethylenediamine flammability, many operation steps, long reaction cycle, etc., to reduce steps and simplify the process , the effect of convenient operation

Pending Publication Date: 2022-07-29
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above synthetic methods all require two-step reactions to synthesize the target product, and intermediate products are produced, and there are many operation steps, which are relatively cumbersome
In addition, the reaction time is longer and the reaction cycle is longer
And the price of catalyst copper-copper oxide or basic copper carbonate used in the reaction is expensive, and the cost is higher
In addition, the reaction raw material ethylenediamine is flammable, and there is a danger of burning and explosion when exposed to open flames, high heat or contact with oxidants, and it is highly corrosive and irritating, which can cause burns to the human body, which makes the operation more dangerous and is not suitable for use in industrial production

Method used

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  • Microwave-assisted rapid synthesis method of N-1-naphthyl ethylenediamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The method for microwave-assisted rapid synthesis of N-1-naphthylethylenediamine hydrochloride comprises the following steps:

[0039] Accurately weigh 1.60 g (0.012 mol) of purchased ethylenediamine hydrochloride and 1.63 g (0.01 mol) of 1-chloronaphthalene, put the former into a round-bottomed flask, and put the latter into a self-made atomizer. A dense mist of 1-chloronaphthalene was regularly sprayed into the bottom flask. When the mist was thick, the 1-chloronaphthalene was continuously sprayed for a period of time until the spraying was completed. Then shake for a few minutes until well mixed and transfer to a sealed reactor. The microwave reactor was set at 300MHz and the rated power was 450W, and the microwave-assisted reaction was started. After the reaction for 1 h, the reaction was stopped, and the reaction was naturally placed and cooled. The solution was transferred to a distillation apparatus for distillation under reduced pressure, and ethylenediamine hy...

Embodiment 2

[0045] The method for microwave-assisted rapid synthesis of N-1-naphthylethylenediamine hydrochloride comprises the following steps:

[0046] Accurately weigh 2.00 g (0.015 mol) of purchased ethylenediamine hydrochloride and 1.63 g (0.01 mol) of 1-chloronaphthalene, put the former into a round-bottomed flask, and put the latter into a self-made atomizer. A dense mist of 1-chloronaphthalene was regularly sprayed into the bottom flask. When the mist was thick, the 1-chloronaphthalene was continuously sprayed for a period of time until the spraying was completed. Then shake for a few minutes until well mixed and transfer to a sealed reactor. The microwave reactor was set at 400MHz and the rated power was 450W, and the microwave-assisted reaction was started. After the reaction for 0.8h, the reaction was stopped, and the reaction was naturally placed and cooled. The solution was transferred to a distillation apparatus for distillation under reduced pressure, and ethylenediamine h...

Embodiment 3

[0051] The method for microwave-assisted rapid synthesis of N-1-naphthylethylenediamine hydrochloride comprises the following steps:

[0052] Accurately weigh 2.66 g (0.020 mol) of purchased ethylenediamine hydrochloride and 1.63 g (0.01 mol) of 1-chloronaphthalene, put the former into a round-bottomed flask, and put the latter into a self-made atomizer. A dense mist of 1-chloronaphthalene was regularly sprayed into the bottom flask. When the mist was thick, the 1-chloronaphthalene was continuously sprayed for a period of time until the spraying was completed. Then shake for a few minutes until well mixed and transfer to a sealed reactor. The microwave reactor was set at 500MHz and the rated power was 450W, and the microwave-assisted reaction was started. After the reaction for 0.5h, the reaction was stopped, and the reaction was naturally placed and cooled. The solution was transferred to a distillation apparatus for distillation under reduced pressure, and ethylenediamine h...

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Abstract

The invention relates to a method for rapidly synthesizing N-1-naphthyl ethylenediamine hydrochloride by a microwave-assisted one-pot method. According to the method, a self-made atomizer is adopted, liquid 1-chloronaphthalene is sprayed to the surface of ethylenediamine hydrochloride solid, the liquid 1-chloronaphthalene is subjected to full contact reaction under microwave radiation, one-pot synthesis is adopted, intermediate products are not generated, and the method has the advantages of being simple in reaction equipment, easy to operate, high in yield and the like. No catalyst is added in the whole process, and the method has the advantages of greenness, no pollution and the like.

Description

technical field [0001] The invention relates to the technical field of preparation and purification of organic compounds, in particular to a method for rapidly synthesizing N-1-naphthylethylenediamine hydrochloride by a microwave-assisted one-pot method. Background technique [0002] The molecular formula of N-1-naphthylethylenediamine hydrochloride is C 12 H 14 N 2 HCl with a molecular weight of 222.5 and a density of 1.36 g / cm 3 , it is usually colorless crystal, melting point is 188~190 ℃, boiling point is 370.7 ℃ at 760 mmHg, flash point is 209.7 ℃, soluble in hot water, ethanol and dilute hydrochloric acid, slightly soluble in cold water, acetone and absolute ethanol. [0003] As a detection reagent, N-1-naphthylethylenediamine hydrochloride has been widely used in many fields such as environment, medicine and food. [0004] In the environmental field, N-1-naphthylethylenediamine hydrochloride can be used as an environmental detection reagent for the detection of ni...

Claims

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Application Information

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IPC IPC(8): C07C209/10C07C209/84C07C209/86C07C211/58
CPCC07C209/10C07C209/84C07C209/86C07C211/58
Inventor 刘娥建方方刘会玲靳泽森李明
Owner HENAN UNIV OF SCI & TECH
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