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Method for preparing dibutylmagnesium

A technology of dibutylmagnesium and n-butyllithium, applied in directions such as magnesium organic compounds, can solve problems such as difficulty in preparing dibutylmagnesium, mercury pollution, production restrictions, etc., achieve favorable environmental protection, simple and effective preparation process, low cost effect

Inactive Publication Date: 2009-02-11
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Because dioxane itself is alkaline, this reaction cannot be completed in an alkali-free environment. Therefore, due to the difficulty in preparing dibutylmagnesium, mercury pollution and must be completed in an alkaline environment, its production is greatly restricted.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Introduce nitrogen into a 250ml four-neck flask reactor equipped with a stirrer, dropping funnel, thermometer, nitrogen inlet tube, and reflux condenser (drying tube on top), heat to drive off water vapor, and remove the heat source after reaching 100°C. When the temperature drops to about 70°C, add 3.65g (0.15mol) of magnesium powder, 2g of 2-chlorobutane, 30mL of ether and a grain of iodine, and stir slowly to make the materials in the reactor reflux stably for 10-20 minutes, and control the temperature at Around 34°C. The liquid in the reactor turns brown. After the reddish brown fades, slowly add 2-chlorobutane solution dropwise. The 2-chlorobutane solution is made by mixing 15g 2-chlorobutane and 110mL ether; control the reaction temperature at 33°C ~35°C, after the dropwise addition, continue to stir and react for 3 hours, then quickly add 60mL n-hexane solution containing 2.5mol / L n-butyllithium to the reactor, reduce the stirring speed, and control the reaction ...

Embodiment 2

[0035]Introduce nitrogen into a 250ml four-neck flask reactor equipped with a stirrer, dropping funnel, thermometer, nitrogen inlet tube, and reflux condenser (drying tube on top), heat to drive off water vapor, and remove the heat source after reaching 100°C. When the temperature drops to about 70°C, add 3.65g (0.15mol) of magnesium powder, 2g of 2-chlorobutane, 30mL of n-hexane and a grain of iodine, stir slowly, and control the temperature at about 65°C. The liquid in the bottle turns rose red. After the rose red fades, slowly add 2-chlorobutane solution dropwise. The 2-chlorobutane solution is made by mixing 15g 2-chlorobutane and 110mL n-hexane; 68°C, continue to stir and react for 3 hours, then quickly add 60mL of n-hexane solution containing 2.5mol / L n-butyl lithium to the reactor, reduce the stirring speed, and control the reaction temperature to 0°C-5°C. After the reaction was completed and separated by filtration, the filtrate was analyzed for Mg content with EDTA, a...

Embodiment 3

[0037] Introduce nitrogen into a 250ml four-neck flask reactor equipped with a stirrer, dropping funnel, thermometer, nitrogen inlet tube, and reflux condenser (drying tube on top), heat to drive off water vapor, and remove the heat source after reaching 100°C. When the temperature drops to about 70°C, add 4.4g (0.18mol) of magnesium powder, 3g of 2-chlorobutane, 100mL of ether and iodine, stir slowly, and control the temperature at about 33°C. The liquid in the bottle turns reddish brown. After the reddish brown fades, slowly add 2-chlorobutane solution dropwise. The 2-chlorobutane solution is prepared by mixing 14g 2-chlorobutane and 160mL ether. The reaction temperature was controlled at 33°C to 35°C, and the stirring reaction was continued for 3 hours, then 60 mL of n-hexane solution containing 2.5 mol / L n-butyllithium was quickly added to the reactor, the stirring speed was reduced, and the reaction temperature was controlled at 0°C to 5 ℃. The reaction was separated by ...

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Abstract

The invention relates to a preparation method for synthesizing dibutyl magnesium by taking 2-chlorobutane, magnesium powder and n-butyl lithium as raw materials. The 2-chlorobutane, the magnesium powder and the n-butyl lithium are taken as raw materials, and the dibutyl magnesium is synthesized under the condition of no water and no oxygenated solvent; the reaction process comprises: under the protection of N2, the magnesium powder is mixed with an evocating agent, then the mixture is put in a reaction kettle for heating and stirring and is added with a small amount of 2-chlorobutane solution slowly; after evocating reaction, under the condition of thermal insulation, the 2-chlorobutane solution is added into the reaction kettle slowly to generate a Grignard reagent by reaction; cooling and temperature reduction are carried out, n-butyl lithium hexane solution is added rapidly; after the reaction under the condition of thermal insulation is carried out, a solvent is obtained by distilling and separating; cooling and filtering are carried out, thus obtaining the dibutyl magnesium; in the preparation process, the mixture ratio of each raw material is as follows: the mole ratio of the magnesium powder to 2-chlorobutane to n-butyl lithium is equal to 1.0-1.2: 1: 1. The preparation method has the advantages of simple and easy technique, no pollution, being investment-saving, high magnesium powder conversion rate and product yield, etc.

Description

technical field [0001] The invention relates to a preparation method for synthesizing dibutyl magnesium by using 2-chlorobutane, magnesium powder and n-butyl lithium as raw materials. Background technique [0002] Organic magnesium halides, or Grignard reagents, are widely used in chemical reactions. Compared with Grignard reagents, dialkylmagnesium reacts similarly to organomagnesium halides and has much fewer applications. The main reason is that so far there is no suitable method for mass production of dialkylmagnesium. Compared with Grignard reagent and alkyllithium, dialkylmagnesium has lower raw material cost and easier transportation. In particular, dialkylmagnesium has excellent chemical properties. Compared with alkyllithium, dialkylmagnesium has better thermal stability and weak ignition (ether solution). Dialkylmagnesium can even be used as a stabilizer for alkyllithium hydrocarbon solutions. Compared with organomagnesium halides, dialkylmagnesiums have strong...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/02
Inventor 吴广文陶凌云吴元欣黄艳刚孙炜朱少坤宋刚张春桂杨峻丁墩墩刘旋
Owner WUHAN INSTITUTE OF TECHNOLOGY
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