Preparation method of 1-bromonaphthalene

A technology of brominated naphthalene and hydrobromic acid, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of high production energy consumption, violent reaction, and large energy consumption, and achieve less reaction by-products , The effect of simple reaction device and low production energy consumption

Inactive Publication Date: 2019-04-19
SHANGHAI WOKAI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The disadvantages of the above methods are: violent reaction, poor temperature control, high risk, strong acid by-products will be produced in the reaction process, long reaction time, a large amount of waste gas containing bromine will be produced, and the energy consumption will be large
[0007] It can be seen that the current method for chemically preparing 1-bromonaphthalene has certain defects, the technology is backward, the production energy consumption is large, and the pollution is serious

Method used

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  • Preparation method of 1-bromonaphthalene

Examples

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Comparison scheme
Effect test

Embodiment 1

[0022] The method that present embodiment prepares 1-bromonaphthalene is as follows:

[0023]

[0024] (1) Get the refined naphthalene of 1mol, be fully dissolved in the ethylene dichloride, then in the stirring process, the hydrobromic acid of 1.1mol is mixed in the solution of ethylene dichloride and naphthalene to form a mixed solution;

[0025] (2) In the process of constant stirring, gradually drop 1.05mol sodium hypochlorite and the above mixed solution under the condition of 30°C;

[0026] (3) After the dropwise addition is completed, stir and keep warm for 60 minutes, then let stand to separate layers, separate the oil phase layer, and then wash it twice to obtain the crude product of the oil phase;

[0027] (4) drying, and then fractional distillation under reduced pressure to obtain 1-bromonaphthalene (yield 95%).

Embodiment 2

[0029] The method that present embodiment prepares 1-bromonaphthalene is as follows:

[0030] (1) Get the refined naphthalene of 1mol, fully dissolve in the ethylene dichloride, then in the stirring process, the hydrobromic acid of 1.05mol is mixed in the solution of ethylene dichloride and naphthalene to form a mixed solution;

[0031] (2) In the process of constant stirring, gradually drop 1.1mol sodium hypochlorite and the above mixed solution under the condition of 25°C;

[0032] (3) After the dropwise addition is completed, stir and insulate for 90 minutes, then stand for stratification, separate the oil phase layer, and then wash it twice to obtain the crude product of the oil phase;

[0033] (4) drying, and then fractional distillation under reduced pressure to obtain 1-bromonaphthalene (yield 96%).

Embodiment 3

[0035] The method that present embodiment prepares 1-bromonaphthalene is as follows:

[0036] (1) Get the refined naphthalene of 1mol, be fully dissolved in the ethylene dichloride, then in the stirring process, the hydrobromic acid of 1.1mol is mixed in the solution of ethylene dichloride and naphthalene to form a mixed solution;

[0037] (2) In the process of constant stirring, gradually drop 1.1mol sodium hypochlorite and the above mixed solution under the condition of 28°C;

[0038] (3) After the dropwise addition is completed, stir and insulate for 70 minutes, then let stand for stratification, separate the oil phase layer, and then wash it twice to obtain the crude product of the oil phase;

[0039] (4) drying, and then fractional distillation under reduced pressure to obtain 1-bromonaphthalene (yield 95%).

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Abstract

Belonging to the technical field of chemical synthesis, the invention specifically relates to a preparation method of 1-bromonaphthalene. The method includes: (1) dissolving naphthalene fully in dichloroethane, and adding hydrobromic acid under stirring to form a mixed solution; (2) adding sodium hypochlorite into the mixed solution dropwise at 25-30DEG C, and conducting heat preservation stirring; (3) carrying out standing layering, taking the oil phase layer, and performing washing; and (4) conducting drying, and performing reduced pressure fractionation, thus obtaining 1-bromonaphthalene. The synthesis process adopted by the invention has the advantages of simple reaction device, few by-product, high yield, high utilization rate of bromine compared with other processes, low pollution ofthree wastes, low production energy consumption, high safety of the reaction process, and conforms to the green chemistry concept.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of 1-bromonaphthalene. Background technique [0002] 1-bromonaphthalene, also known as 1-bromonaphthalene, A-bromonaphthalene, is a colorless or slightly yellow liquid, which can remain colorless after distillation, but turns black after a long time. Compatible with alcohol, ether, carbon tetrachloride, insoluble in water. With water vapor can be volatile. It can be used as raw material for organic synthesis, analytical reagent, refrigerant and solvent for substances with large molecular weight. It is also a heat carrier for drying items. It can also be used for refractive index determination. The high magnification objective lens (100X) of the optical microscope uses bromonaphthalene as the refractive medium, and increases the numerical aperture of the objective lens to increase the magnification. [0003] The conventional method ...

Claims

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Application Information

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IPC IPC(8): C07C17/12C07C25/22
CPCC07C17/12C07C25/22
Inventor 柯德宏郭建国薛循育陆惠懿
Owner SHANGHAI WOKAI BIOTECH
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