Preparation method of tert-butyllithium solution

A technology of tert-butyllithium and solution, applied in the field of basic chemical industry, can solve the problems of not getting the target product, the success rate is low, and the reaction is difficult to initiate, and achieves the effects of controlling the content of impurities, improving the success rate, and ensuring quality

Active Publication Date: 2013-04-17
SHANGYU HUALUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, n-butyllithium can be prepared on a large scale in industry, while tert-butyllithium can only be prepared on a small scale in the laboratory because it is too active and its raw materials are relatively stable. When it is scaled up to an industrial scale, The reaction is often difficult to initiate, the success rate is low, and the target product cannot be obtained

Method used

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  • Preparation method of tert-butyllithium solution

Examples

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Embodiment 1

[0026] Under argon protection, 21 g of 3% sodium-lithium alloy and 150 ml of high-boiling inert solvent (white oil) were added to a 1 L three-necked flask equipped with a high-speed stirrer. After replacing the air in the system with argon, slowly start stirring and heat to 200°C to completely melt the metal. At this time, the stirring speed rises to 1200r / min and the temperature reaches 210°C. Stir at high speed for 10 minutes at this temperature. Stop heating and stirring, and place the reaction bottle in a cold water bath to cool it down as soon as possible. After the temperature drops to 90°C, start stirring to further cool down to room temperature. The solvent was pressure filtered off under a flow of argon and washed three times with sodium-treated pentane. Finally, under the protection of argon, the solvent was evaporated to dryness, 470ml of dry pentane was added and heated to reflux the pentane, and 107ml (0.979mol) of chloro-tert-butane was added dropwise under vigor...

Embodiment 2

[0028] Under the protection of argon, 21 g of 3% sodium-lithium alloy and 150 ml of high-boiling inert solvent (white oil) were added to a 1 L three-necked flask equipped with a high-speed stirrer. After replacing the air in the system with argon, slowly start stirring and heat to 200°C to completely melt the metal. At this time, the stirring speed rises to 1200r / min and the temperature reaches 210°C. Stir at high speed for 10 minutes at this temperature. Stop heating and stirring, and place the reaction bottle in a cold water bath to cool it down as soon as possible. After the temperature drops to 90°C, start stirring to further cool down to room temperature. The solvent was pressure filtered under argon flow and washed three times with sodium treated n-hexane. Finally, under the protection of argon, the solvent was evaporated to dryness, 470ml of dry n-hexane was added and heated to reflux the n-hexane, and 107ml (0.979mol) of chloro-tert-butane was dripped under vigorous st...

Embodiment 3

[0030] Under argon protection, add 21 g of lithium and 150 ml of high-boiling inert solvent (white oil) into a 1 L three-necked flask equipped with a high-speed stirrer. After replacing the air in the system with argon, slowly start stirring and heat to 200°C to completely melt the metal. At this time, the stirring speed increases to 1200r / min, and the temperature reaches 205°C. Stir at high speed for 10 minutes at this temperature. Stop heating and stirring, and place the reaction bottle in a cold water bath to cool it down as soon as possible. After the temperature drops to 90°C, start stirring to further cool down to room temperature. The solvent was pressure filtered under argon flow and washed three times with sodium treated n-hexane. Finally, under the protection of argon, the solvent was evaporated to dryness, 470ml of dry pentane was added and heated to reflux the pentane, and 107ml (0.979mol) of chloro-tert-butane was dripped under vigorous stirring. The reaction coul...

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Abstract

The invention discloses a preparation method of a tert-butyllithium solution, which comprises the following steps: (1) in an inert gas protective atmosphere, adding sodium-lithium alloy into an inert solvent, heating while stirring to disperse the sodium-lithium alloy, cooling, and removing the inert solvent to obtain a sodium-lithium alloy dispersion; and (2) in an inert gas protective atmosphere, adding pentane into the sodium-lithium alloy dispersion obtained in the step (1), dropwisely adding a chlorinated n-butane-chlorinated tert-butyl alkane mixed solution at 30-38 DEG C while stirring to carry out reaction, and after the reaction is complete, treating to obtain the tert-butyllithium solution. By adding the catalytic amount of chlorinated n-butane into chlorinated tert-butyl alkane, the reaction for preparing the tert-butyllithium can be initiated and carried out smoothly, thereby implementing industrialized-scale production of the tert-butyllithium.

Description

technical field [0001] The invention belongs to the field of basic chemical industry, and in particular relates to a preparation method of a tert-butyllithium solution. Background technique [0002] Organolithium compounds are an important class of organometallic compounds. As early as 1929, K. Ziegler prepared them by reacting organic halides with metal lithium, and then applied them in organic synthesis. At present, organolithium compounds, as an important synthetic reagent, play an important role in basic theoretical research and industrial synthesis. [0003] The chemical properties of organolithium compounds are similar to alkylmagnesium halides, but they are more active and can react with metal halides, carbonyl-containing substances, halogenated hydrocarbons and compounds containing active hydrogen. Commonly used organolithium compounds include butyllithium and phenyllithium, among which butyllithium is mainly used to remove active hydrogen in organic compounds. But...

Claims

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Application Information

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IPC IPC(8): C07F1/02C07D407/04
Inventor 李典正张江林何光明
Owner SHANGYU HUALUN CHEM
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