A kind of synthetic method of 2,5-dibromoiodobenzene

A technology of dibromoiodobenzene and its synthesis method, which is applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of raw material monopoly, monopoly, unfavorable scale and popularization of industrial production, and achieve The effect of large quantity and low cost

Active Publication Date: 2021-03-12
鹤壁市海格化工科技有限公司
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem in the prior art that only 1,4-dibromobenzene can be used to prepare 2,5-dibromoiodobenzene, which is too single, and it is easy to cause monopoly of raw materials in industrial production. The shortcoming that is conducive to the large-scale development of industrial production and the popularization development, and proposes a kind of synthetic method of 2,5-dibromoiodobenzene

Method used

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  • A kind of synthetic method of 2,5-dibromoiodobenzene

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Embodiment 1

[0021] A kind of synthetic method of 2,5-dibromoiodobenzene that the present invention proposes, comprises the following steps: S1, the synthesis of 2-nitro-4-bromophenol: add p-bromophenol in chemical reaction still, then under room temperature condition Add dilute nitric acid directly under the pressure, let it stand for 20min, carry out fractional distillation of the reactant under reduced pressure, collect 125°C, 2.35kPa fraction to obtain 2-nitro-4-bromophenol;

[0022] S2, the synthesis of 2-amino-4-bromophenol: put 2-nitro-4-bromophenol in a chemical reaction kettle, add Fe and dilute HCl to 2-nitro-4-bromophenol, and carry out Heating to realize ortho-position nitration, keeping the temperature at 70°C for 1 hour, fractionating the reactant under reduced pressure, collecting fractions at 105°C and 2.57kPa to obtain 2-amino-4-bromophenol;

[0023] Synthesis of S3, 2-iodo-4-bromophenol: add a little excess NaNO to the reaction kettle 2 , HI, then add 2-amino-4-bromophen...

Embodiment 2

[0026] A kind of synthetic method of 2,5-dibromoiodobenzene that the present invention proposes, comprises the following steps: S1, the synthesis of 2-nitro-4-bromophenol: add p-bromophenol in chemical reaction still, then under room temperature condition Add dilute nitric acid directly under the pressure, let it stand for 30min, carry out fractional distillation of the reactant under reduced pressure, collect 125°C, 2.35kPa fraction to obtain 2-nitro-4-bromophenol;

[0027] S2, the synthesis of 2-amino-4-bromophenol: put 2-nitro-4-bromophenol in a chemical reaction kettle, add Fe and dilute HCl to 2-nitro-4-bromophenol, and carry out Heating to realize ortho nitration, the temperature is kept at 75°C for 1.5h, the reactant is fractionated under reduced pressure, and the fraction at 110°C and 2.63kPa is collected to obtain 2-amino-4-bromophenol;

[0028] Synthesis of S3, 2-iodo-4-bromophenol: add a little excess NaNO to the reaction kettle 2 , HI, then add 2-amino-4-bromophen...

Embodiment 3

[0031] A kind of synthetic method of 2,5-dibromoiodobenzene that the present invention proposes, comprises the following steps: S1, the synthesis of 2-nitro-4-bromophenol: add p-bromophenol in chemical reaction still, then under room temperature condition Add dilute nitric acid directly under the pressure, let it stand for 35min, carry out fractional distillation under reduced pressure, collect 130°C, 2.95kPa distillate to obtain 2-nitro-4-bromophenol;

[0032] S2, the synthesis of 2-amino-4-bromophenol: put 2-nitro-4-bromophenol in a chemical reaction kettle, add Fe and dilute HCl to 2-nitro-4-bromophenol, and carry out Heating to realize ortho nitration, keeping the temperature at 80°C for 1.5h, fractionating the reactant under reduced pressure, collecting fractions at 120°C and 2.73kPa to obtain 2-amino-4-bromophenol;

[0033] Synthesis of S3, 2-iodo-4-bromophenol: add a little excess NaNO to the reaction kettle 2 , HI, then add 2-amino-4-bromophenol, keep the temperature ...

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Abstract

The invention discloses a synthesis method of 2,5-dibromoiodobenzene, comprising the following steps: S1, synthesis of 2-nitro-4-bromophenol; S2, synthesis of 2-amino-4-bromophenol; The synthesis of S3, 2-iodine-4-bromophenol; the synthesis of S4, 2,5-dibromoiodobenzene: 2-iodine-4-bromophenol is placed in a chemical reaction kettle, and then dioxane solvent is added, And stir at room temperature, gradually add phosphorus tribromide in this process, reactant is subjected to vacuum fractionation, collects 130-140 ℃, 3.25-3.45kPa fraction promptly obtains 2,5-dibromoiodobenzene, the present invention Utilize p-bromophenol as raw material, carry out the preparation of 2-nitro-4-bromophenol by p-bromophenol, then further prepare 2-amino-4-bromophenol, and then turn into 2-iodo-4-bromophenol , finally synthesized 2,5-dibromoiodobenzene, realized the synthesis and preparation of 2,5-dibromoiodobenzene in another way, expanded the preparation raw materials of 2,5-dibromoiodobenzene, and simultaneously the raw material parabromo Phenol is low in cost and large in quantity, making it convenient for industrial production.

Description

technical field [0001] The invention relates to the technical field of 2,5-dibromoiodobenzene, in particular to a synthesis method of 2,5-dibromoiodobenzene. Background technique [0002] 2,5-Dibromoiodobenzene is a very important raw material for fine chemicals. It is a halogenated benzene and is a white solid. It is mainly used in the synthesis of medicines, pesticides, dyes, plastics and functional polymer materials. At present, the preparation method of 2,5-dibromoiodobenzene reported in the literature at home and abroad is mainly based on 1,4-dibromobenzene as the starting material, in organic solvents such as tetrahydrofuran, through tetramethylpiperidinyl Lithium reacts, and then continues to react with iodine simple substance to obtain 2,5-dibromoiodobenzene (European Journal of Organic Chemistry, (10), 1797-1801; 2008). However, the method of preparing 2,5-dibromoiodobenzene by simply using 1,4-dibromobenzene is too single, which easily leads to the monopoly of raw...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/16C07C25/02
CPCC07C17/16C07C37/05C07C201/10C07C209/365C07C205/12C07C211/52C07C39/27C07C25/02
Inventor 房忠雪王羽詹浩晟胡志伟
Owner 鹤壁市海格化工科技有限公司
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