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Preparation method of 3, 5-dibromo iodobenzene

A technology of dibromoiodobenzene and iodoaniline, applied in 3 fields, can solve problems such as many by-products, high toxicity, long reaction steps, etc., and achieves the effects of improving yield, easy operation and control, and being beneficial to industrialized production

Inactive Publication Date: 2016-04-27
SHANGHAI HUAXIAN NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the reaction steps are long, the by-products are many, and the toxicity is high.

Method used

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  • Preparation method of 3, 5-dibromo iodobenzene
  • Preparation method of 3, 5-dibromo iodobenzene
  • Preparation method of 3, 5-dibromo iodobenzene

Examples

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Embodiment 1

[0020] 3 of the present invention, the preparation method of 5-dibromoiodobenzene comprises the following steps:

[0021] Step 1, the preparation step of 2,6-dibromo-4-iodoaniline intermediate, add p-iodoaniline and absolute ethanol in a container, under normal temperature conditions, add dibromohydantoin in batches; no raw materials are detected by HPLC When the product is produced, stop the reaction; directly filter to obtain the 2,6-dibromo-4-iodoaniline intermediate; the molar ratio of p-iodoaniline to dibromohydantoin is 1:1.

[0022] Step 2, add 2-, 6-dibromo-4-iodoaniline intermediate and hypophosphorous acid in another container, add sodium nitrite solution dropwise after cooling down, a large amount of solids will wash out after dropping, filter directly , recrystallized from absolute ethanol to obtain needle-like 3,5-dibromoiodobenzene. The molar ratio of 2,6-dibromo-4-iodoaniline intermediate to sodium nitrite is 1:1.

[0023] Preparation of intermediate 2,6-dibro...

Embodiment 2

[0030] The preparation of intermediate 2,6-dibromo-4-iodoaniline: the detailed steps are as follows: wherein, the dosage is as follows: p-iodoaniline: 219g, dibromohydantoin: 290g, absolute ethanol: 1800ml. Add 219g of p-iodoaniline (1mol) and 1000ml of absolute ethanol into a 2000ml reaction bottle, stir for 20 minutes to disperse evenly. Then add 290 g of dibromohydantoin in batches, control the reaction temperature at 20-25° C., and complete the addition in about 2 hours. After the addition, a large amount of white solids will precipitate out. Reaction was continued at this temperature for 1 hour. The reaction was monitored by HPLC. When the raw materials disappeared, the reaction was stopped, filtered at 20-25°C, and dried under normal pressure at 100°C to obtain 350 g of off-white powdery solid. like image 3 And the HPLC collection of illustrative plates of 2,6-dibromo-4-iodoaniline shown in Table 3, collection of illustrative plates shows 2,6-dibromo-4-iodoaniline con...

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Abstract

The present invention discloses a preparation method of 3, 5-dibromo iodobenzene. The preparation method comprises the following steps: Step 1, p-Iodoaniline and absolute ethyl alcohol are added into a container, and dibromodimethyl hydantoin is added into the container in batches at room temperature; a reaction is stopped until no raw material product is detected by HPLC spectrum; and a 2,6-dibromo-4-iodoaniline intermediate can be obtained by a direct filtration; and Step 2, the 2,6-dibromo-4-iodoaniline intermediate and hypophosphorous acid are added into another container, sodium nitrite solution is dropwise added into the container after the container is cooled, solids are washed out at the end of the dropwise addition process, and after direct filtration, acicular 3,5-dibromo iodobenzene can be obtained by recrystallization in absolute ethyl alcohol. The preparation method improves the production and operation environment, and uses cheap 1-Bromo-3-chloro-5,5-dimethylimidazolidine-2,4-dione as a solvent for product preparation, is easy to operate and control, improves yields, shortens reaction time, reduces costs, and is beneficial to industrial production.

Description

technical field [0001] The invention relates to a preparation method of dibromoiodobenzene, in particular to a preparation method of 3,5-dibromoiodobenzene. Background technique [0002] 3,5-Dibromoiodobenzene is an important organic intermediate widely used in the fields of dyes, pigments, medicines and pesticides. At present, the general synthesis methods are: amidation of aniline, and then bromination, iodination reaction, and then deprotection and deamination. The disadvantage of this method is that the reaction steps are long, the by-products are many, and the toxicity is high. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a method for preparing 3,5-dibromoiodobenzene which is economical and simple, has mild reaction conditions, good operating environment, high yield and high purity. [0004] The present invention solves the above-mentioned technical problems through the following technical scheme: a kin...

Claims

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Application Information

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IPC IPC(8): C07C25/02C07C17/35
Inventor 吴跃初宋文志林亚飞
Owner SHANGHAI HUAXIAN NEW MATERIAL TECH CO LTD
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