Bromination reaction method

A technology of bromination reaction and reaction formula, which is applied in the field of organic synthesis, can solve problems such as unfavorable large-scale industrial production, influence of target product yield, and bromination reaction does not avoid water, so as to improve the production environment, facilitate separation, and reduce consumption Effect

Active Publication Date: 2013-04-03
山西新天源药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the main limitation of this method is that it is required that the bromination reaction should not avoid water, and the reaction raw materials and products are not easy to be oxidized, otherwise the yield of the target product will be greatly affected; in addition, this method will produce 2 , HBr and H 2 o 2 waste water, the treatment of this waste water is also a difficult problem
[0009] It can be seen that greatly improving the utilization rate of bromine is the only way to improve the economy of bromination reaction, but there are still many defects in the reported bromination reaction method, which is not conducive to large-scale industrial production

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0026] Example 1: Preparation of m-bromonitrobenzene.

[0027] Take 16.8kg of liquid bromine in the bromine metering tank 3 for use; add three-quarters of the volume to the bromine regeneration tank 2 with condenser 5 containing 25% free SO 3 To maintain the temperature of the bromine regeneration tank 2 at 35℃~60℃.

[0028] Take 26.4kg of freshly steamed nitrobenzene and 0.2kg of iron powder into the brominated reaction tank 1 with condenser 5, stir evenly, raise the temperature of the oil bath to 135℃~145℃, and put the bromine metering tank 3 under rapid stirring. The liquid bromine in the bromine is slowly injected into the bromine reaction tank 1 from the bottom through the flow meter 4, and the injection rate is at the level of the substantially bromine-free steam overflow. The overflowing hydrogen bromide gas is passed into the fuming sulfuric acid in the bromine regeneration tank 2 through the pipe In the regeneration.

[0029] After the liquid bromine in the bromine metering...

Embodiment 2

[0032] Example 2: Preparation of 9-bromophenanthrene.

[0033] Take 16.6kg of liquid bromine and put it in the bromine metering tank 3 for use; add three-quarters of the volume to the bromine regeneration tank 2 with condenser 5 containing 20% ​​free SO 3 To maintain the temperature of the bromine regeneration tank 2 at 35℃~60℃.

[0034] Take 35.6kg of refined phenanthrene, 0.1kg of iodine, and 70L of dry carbon tetrachloride into the brominated reaction tank 1 with condenser 5, stir well, and raise the temperature to slightly boiling. Under rapid stirring, the liquid bromine in the bromine metering tank 3 is slowly injected into the brominated reaction tank 1 from the bottom through the flow meter 4, and the injection rate is to maintain the slightly boiling of the reaction liquid. The overflowing hydrogen bromide gas is introduced through the pipe The bromine regeneration tank 2 is regenerated in fuming sulfuric acid.

[0035] After the liquid bromine in the bromine metering tank ...

Embodiment 3

[0038] Example 3: Preparation of tetrabromoparaene.

[0039] Take 67.5kg of liquid bromine and put it in the bromine metering tank 3 for use; add three-quarters of the volume to the bromine regeneration tank 2 with condenser 5 containing 40% free SO 3 To maintain the temperature of the bromine regeneration tank 2 at 35℃~60℃.

[0040] Take 21.2 kg of o-xylene and 100 L of dry carbon tetrachloride into the brominated reaction tank 1 with condenser 5, stir evenly, and raise the temperature to reflux. Stir quickly and under the irradiation of a 500W ultraviolet lamp, the liquid bromine in the bromine metering tank 3 is slowly injected into the bromine reaction tank 1 from the bottom through the flow meter 4, and the injection rate is basically no bromine overflow, and the overflowing bromine The hydrogen gas is passed into the fuming sulfuric acid in the bromine regeneration tank 2 through the pipe for regeneration.

[0041] After the liquid bromine in the bromine metering tank 3 is add...

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Abstract

The invention discloses a bromination reaction method, which is realized through performing bromination reaction and bromine regeneration reaction in a separating way and recycling bromine, that is, the bromine is led into an independent bromination reaction container, and is in bromination reaction with bromo reactant therein, produced hydrogen bromide gas is led into an independent bromine regeneration container via a duct, and reacted with a bromine regeneration solution therein to produce bromine, and then the bromine is led into the bromination reaction container over again to perform bromination reaction until the bromination reaction is finished completely through circulation. The bromination reaction method provided by the invention has no loss of bromine in the whole process, and is simple and convenient, economic, green and environment-friendly, and the utilization ratio of bromine is up to more than 97 percent.

Description

Technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a bromination reaction method, in particular to a bromination reaction method using bromine as a bromination reagent. Background technique [0002] Bromination reaction is one of the most common organic synthesis unit reactions. Most of the fine chemical products containing bromine are prepared through bromination reaction. The reaction scheme is as follows. [0003] [0004] Where R 1 Can be: hydrogen (-H), hydroxyl (-OH), diazonium salt (-N 2 + X - ), metal ions (-M n+ ),Wait. [0005] The difference in bromination reactions is mainly determined by the different types of brominated reagents used. Commonly used brominated reagents include bromine, hydrobromic acid, hypobromous acid, phosphorus tribromide, phosphorus pentabromide, phosphorus oxybromide, and sulfite Acid bromide, N-bromosuccinimide, N-bromophthalimide, bromide, bromate, etc. Comprehensive comparison, the most wid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B39/00C07C205/12C07C201/12C07C25/22C07C17/12C07C25/02C07C17/14C07C67/307C07C69/63
Inventor 苏斌林汤芝平苏蔚武杰成高志伟康福堂
Owner 山西新天源药业有限公司
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