Preparation method of n-hexyl lithium

A technology of n-hexyllithium and n-hexane, which is applied in the field of organometallic compound synthesis, can solve problems such as reducing the yield of n-hexyllithium, reducing the purity of n-hexyllithium, and affecting applications, so as to improve the conversion rate and reduce the impact of amplification benefits , reduce the effect of side effects

Active Publication Date: 2013-12-11
SHANGYU HUALUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This will not only reduce the yield of n-hexyllithium, but also reduce the purity of n-hexyllithium, affecting subsequent applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Under argon protection, put 250L white oil and 21kg lithium flakes into the 500L reaction kettle, slowly stir and heat up to 180°C, after stirring for 0.5h, speed up the stirring speed of the reaction kettle to 130 rpm, stir at 180°C for 1h, turn on and cool to At room temperature, the white oil was removed by pressure filtration, and the n-hexane was transferred to the washing kettle and rinsed 2-3 times to obtain a relatively uniform lithium metal form (lithium sand).

[0030] Under the protection of argon, add 20kg of n-hexane to the 500L reactor, put in 7kg of lithium sand and 58g of L-proline under the condition that argon is kept in the kettle, cover and maintain positive pressure, open the open valve to maintain pressure balance , add 80kg n-hexane to the reaction kettle, slowly start stirring; be warming up to 55 ℃, open the balance pipe valve, drip 60kg chloro-n-hexane, control the reaction kettle temperature at about 53-55 ℃; control the reaction kettle rotatin...

Embodiment 2

[0040] Under argon protection, put 250L white oil and 21kg lithium flakes into the 500L reaction kettle, slowly stir and heat up to 180°C, after stirring for 0.5h, speed up the stirring speed of the reaction kettle to 130 rpm, stir at 180°C for 1h, turn on and cool to At room temperature, the white oil was removed by pressure filtration, and the n-hexane was transferred to the washing kettle and rinsed 2-3 times to obtain a relatively uniform lithium metal form (lithium sand).

[0041] Under the protection of argon, add 20kg of n-hexane to the 500L reaction kettle, put in 7kg of lithium sand while keeping argon in the kettle, cover and maintain positive pressure, open the open valve to maintain pressure balance, and add 80kg to the reaction kettle. n-hexane, slowly start stirring; be warming up to 55 ℃, open the balance pipe valve, drip 60kg of chloro-n-hexane, control the temperature of the reaction kettle to 53-55 ℃; control the speed of the reaction kettle to be 130 rev / min....

Embodiment 3

[0043]Under argon protection, put 250L white oil and 21kg lithium flakes into the 500L reaction kettle, slowly stir and heat up to 180°C, after stirring for 0.5h, speed up the stirring speed of the reaction kettle to 130 rpm, stir at 180°C for 1h, turn on and cool to At room temperature, the white oil was removed by pressure filtration, and the n-hexane was transferred to the washing kettle and rinsed 2-3 times to obtain a relatively uniform lithium metal form (lithium sand).

[0044] Under the protection of argon, add 20kg of n-hexane to the 500L reaction kettle, put in 7kg of lithium sand while keeping argon in the kettle, cover and maintain positive pressure, open the open valve to maintain pressure balance, and add 80kg to the reaction kettle. n-hexane, slowly start stirring; be warmed up to a slight reflux, open the balance pipe valve, drop 60kg of chloro-n-hexane, control the temperature of the reaction kettle to 65-66 ℃; control the speed of the reaction kettle to be 130...

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Abstract

The invention discloses a preparation method of n-hexyl lithium, which comprises the following steps of (1), placing a lithium sheet in an inert solvent under protection of inert gas, heating and stirring to allow the lithium sheet to be dispersed, cooling, removing the inert solvent, obtaining a lithium dispersoid, and (2), adding a liquid hydrocarbon solvent to the lithium dispersoid obtained in Step (1) under the protection of the inert gas, adding L-proline with a catalytic amount, stirring, heating, flowing back, dropwise adding chlorohexane, reacting completely, and obtaining a solution of n-hexyl lithium through treatment. According to the preparation method, after catalyst L-proline is coordinated with lithium, a yield of a product is increased, and a side reaction is reduced.

Description

technical field [0001] The invention belongs to the field of organometallic compound synthesis, in particular to a preparation method of n-hexyllithium. Background technique [0002] Organolithium compounds are an important class of organometallic compounds, which were prepared by K. Ziegler as early as 1929 by reacting organic halides with metallic lithium, and subsequently 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 those of alkyl magnesium halides, but they are more active and can react with metal halides, carbonyl-containing substances, halogenated hydrocarbons and compounds containing active hydrogen. N-hexyllithium is an important organolithium compound, which can be used to remove the active hydrogen of many hydrogen carbonates, and the more important ap...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07F1/02
Inventor李典正张江林何光明
OwnerSHANGYU HUALUN CHEM