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Production method of 1-bromine-2-butyne

A production method and technology for butyne, applied in the field of organic synthesis, can solve the problems of substrate sensitivity, equipment corrosion and high production cost, and achieve the effects of mild reaction conditions, high utilization rate and low risk

Inactive Publication Date: 2016-12-07
安徽济达化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1) The production of 2-butyn-1-ol mainly adopts the methods of butyllithium, sodium metal and sodium amide. The substrates of these methods are extremely sensitive to external media such as air, and production accidents are prone to occur; at the same time, due to the need for these processes Ultra-low temperature reaction has extremely strict requirements on production equipment, and it is also a major restrictive factor for industrial production
[0004] 2) The by-product of the bromine process, hydrogen bromide, is highly acidic and severely corrodes the equipment. Therefore, a special recovery device is required for processing and recovery during the production process, and the production cost is high.

Method used

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  • Production method of 1-bromine-2-butyne
  • Production method of 1-bromine-2-butyne

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Experimental program
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Effect test

Embodiment 1

[0019] Action 1: Check that all equipment is in normal condition. 90kg of magnesium scraps were added to the 2000L dry reaction kettle, the reaction kettle was evacuated, 150kg of THF was pumped into the reaction kettle, and the stirring mechanism in the reaction kettle was started; a small amount of ethyl bromide was added to the reaction kettle, and the temperature was raised to initiate the reaction (The temperature in the reactor is obviously heated up, and the reflux pipe has the phenomenon of reflux) The remaining 900kgTHF is added to the reactor, and then 360kg of ethyl bromide is added dropwise, and the temperature in the reactor is controlled at 60 ° C; The reaction was carried out for 2h; after the insulation was completed, the reaction kettle was cooled to 5°C, and propyne gas was introduced into the reaction kettle. , 5 ℃ for 12h; the reaction kettle was heated to 45 ℃, and paraformaldehyde was added in batches (about 3-6 kilograms were added every 15 minutes), a t...

Embodiment 2

[0022] Action 1: Check that all equipment is in normal condition. 120kg of magnesium scraps were added into the 2000L dry reaction kettle, the reaction kettle was evacuated, 200kg of THF was pumped into the reaction kettle, and the stirring mechanism in the reaction kettle was started; a small amount of ethyl bromide was added into the reaction kettle, and the temperature was raised to initiate the reaction (The temperature in the reactor is obviously heated up, and the reflux pipe has the phenomenon of reflux) The remaining 1300kgTHF is added to the reactor, then 400kg of ethyl bromide is added dropwise, and the temperature in the reactor is controlled at 40 ° C; The reaction was carried out for 3h; after the insulation was completed, the reaction kettle was cooled to -5°C, and propyne gas was introduced into the reaction kettle. Then, keep the temperature at 15°C for 12h; heat the reaction kettle to 35°C, add paraformaldehyde in batches (about 3-6 kg every 15 minutes), add a...

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Abstract

The invention relates to a production method of 1-bromine-2-butyne. The production method comprises the following steps of enabling ethyl bromide and metal magnesium to be subjected to a reaction in THF so as to obtain a Grignard reagent, then adding paraformaldehyde to the Grignard reagent for performing a Grignard reaction, and after the Grignard reaction is completed, performing separation and recovery of 2-butyne-1-alcohol; and enabling 2-butyne-1-alcohol and phosphorus tribromide to be subjected to a bromination reaction, and after the bromination reaction is completed, performing separation and recovery of the 1-bromine-2-butyne. The Grignard reaction adopted by the production method disclosed by the invention is widely used at present, special production equipment is not needed, reaction conditions are relatively mild, the Grignard reaction is stable in an industrialized production process, and the danger is reduced. The phosphorus tribromide is used for performing bromination on the 2-butyne-1-alcohol, and the utilization rate of the bromine is high; and a generated byproduct namely phosphoric acid is neutralized with pyridine, so that the phosphoric acid is easy to treat.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for producing 1-bromo-2-butyne. Background technique [0002] 1-Bromo-2-butyne is often used to synthesize axial chiral ternary compounds. The production of 1-bromo-2-butyne mainly adopts a two-step method, that is, 2-butyn-1-ol is prepared first, and then bromine The bromination treatment of 2-butyn-1-ol is carried out by the basic process, and this scheme has the following disadvantages. [0003] 1) The production of 2-butyn-1-ol mainly uses butyllithium, sodium metal, and sodium amide methods. The substrates of these methods are extremely sensitive to external media such as air, and production accidents are prone to occur; at the same time, due to the needs of these processes. Ultra-low temperature reaction is extremely demanding on production equipment, and it is also a big constraint on industrial production. [0004] 2) Hydrogen bromide, the by-product of the bro...

Claims

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Application Information

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IPC IPC(8): C07C17/16C07C21/22
CPCC07C17/16C07C29/40C07C21/22C07C33/042
Inventor 毛晓宇黄明辉吴孝增
Owner 安徽济达化工科技有限公司