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

AI Technical Summary

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 produce

Method used

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  • Preparation method of 1-bromonaphthalene

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021] Example 1

[0022] The method for preparing 1-bromonaphthalene in this embodiment is as follows:

[0023]

[0024] (1) Take 1 mol of refined naphthalene, fully dissolve it in dichloroethane, and then mix 1.1 mol of hydrogen bromide into the solution of dichloroethane and naphthalene to form a mixed solution during the stirring process;

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

[0026] (3) After the dripping is completed, stir and keep for 60 minutes, then stand still for layering, divide the oil phase layer, and then wash it twice with water to obtain the crude oil phase;

[0027] (4) Drying and fractionating under reduced pressure to obtain 1-bromonaphthalene (yield 95%).

Example Embodiment

[0028] Example 2

[0029] The method for preparing 1-bromonaphthalene in this embodiment is as follows:

[0030] (1) Take 1 mol of refined naphthalene, fully dissolve it in dichloroethane, and then mix 1.05 mol of hydrobromic acid into the solution of dichloroethane and naphthalene to form a mixed solution during the stirring process;

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

[0032] (3) After the dripping is completed, stir and keep for 90 minutes, then stand still for layering, divide the oil phase layer, and then wash it twice with water to obtain the crude oil phase;

[0033] (4) Drying and fractionating under reduced pressure to obtain 1-bromonaphthalene (yield 96%).

Example Embodiment

[0034] Example 3

[0035] The method for preparing 1-bromonaphthalene in this embodiment is as follows:

[0036] (1) Take 1 mol of refined naphthalene, fully dissolve it in dichloroethane, and then mix 1.1 mol of hydrogen bromide into the solution of dichloroethane and naphthalene to form a mixed solution during the stirring process;

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

[0038] (3) After the dripping is completed, stir and keep for 70 minutes, then stand still for layering, divide the oil phase layer, and wash it twice with water to obtain the crude oil phase;

[0039] (4) Drying and fractionating 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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