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Method for synthesizing an organic zinc compound

A synthesis method and compound technology, applied in the direction of zinc organic compounds, etc., to achieve the effect of simple and easy activation method

Inactive Publication Date: 2010-08-25
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The synthetic method of unsymmetrical organozinc compound, bibliographical report is few at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 2

[0020] The synthesis of embodiment 1 dibutylzinc

[0021] Take a 500ml three-necked bottle, add 6.8g zinc powder, vacuumize and fill with nitrogen. To this was added 8 ml of tetrahydrofuran and a catalytic amount of BrCH 2 CH 2 Br catalyst and catalytic amount of SiMe 3 Cl catalyst to obtain a tetrahydrofuran solution containing activated zinc powder. Add 11.4ml n-butyl iodide and 40ml tetrahydrofuran solvent to it again and stir, obtain containing after the reaction n BuZnI (n-butylzinc iodide) solution in tetrahydrofuran.

[0022] Take another 250ml three-necked flask, add 2.64g of magnesium powder and a catalytic amount of iodine simple substance catalyst, vacuumize it, fill it with nitrogen, and add 20ml of tetrahydrofuran solvent therein. Add 11.9ml n-butyl bromide and 25ml tetrahydrofuran solvent to it again and stir, after reaction, obtain containing n BuMgBr (n-butylmagnesium bromide) solution in tetrahydrofuran.

[0023] To the above obtained containing n BuMg...

Embodiment 2 2

[0024] The synthesis of embodiment 2 diisobutyl zinc

[0025] Take a 500ml three-necked bottle, add 6.8g zinc powder, vacuumize and fill with nitrogen. To this was added 8 ml of tetrahydrofuran and a catalytic amount of BrCH 2 CH 2 Br catalyst and catalytic amount of SiMe 3 Cl catalyst to obtain a tetrahydrofuran solution containing activated zinc powder. Add 11.5ml isobutyl iodide and 40ml tetrahydrofuran solvent to it again and stir, obtain containing after the reaction i BuZnI (isobutylzinc iodide) solution in tetrahydrofuran.

[0026] Take another 250ml there-necked flask, add 2.64g of magnesium powder and a catalytic amount of iodine simple substance catalyst, vacuumize it, fill it with nitrogen, and then add 20ml of ether solvent therein. Add 10.9ml isobutyl bromide and 25ml ether solvent to it again and stir, after the reaction, obtain i BuMgBr (isobutylmagnesium bromide) in THF.

[0027] To the above obtained containing i BuMgBr solution in tetrahydrofuran was ...

Embodiment 3 2

[0028] The synthesis of embodiment 3 diisopropylzinc

[0029] Take a 500ml three-necked bottle, add 6.8g zinc powder, vacuumize and fill with nitrogen. To this was added 8 ml of tetrahydrofuran and a catalytic amount of BrCH 2 CH 2 Br catalyst and catalytic amount of SiMe 3 Cl catalyst to obtain a tetrahydrofuran solution containing activated zinc powder. Add 10ml isopropyl iodide and 40ml tetrahydrofuran solvent to it again and stir, obtain containing after the reaction i PrZnI (isopropylzinc iodide) in tetrahydrofuran.

[0030] Take another 250ml there-necked flask, add 2.64g of magnesium powder and a catalytic amount of iodine simple substance catalyst, vacuumize it, fill it with nitrogen, and then add 20ml of ether solvent therein. Add 9.4ml isopropyl bromide and 25ml ether solvent to it again and stir, after the reaction, obtain containing i PrMgBr (isopropylmagnesium bromide) in tetrahydrofuran.

[0031] To the above obtained containing i The tetrahydrofuran solu...

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Abstract

The invention relates to a method for synthesizing an organic zinc compound. The method directly starts from zinc powder and comprises the following steps of: activating the zinc powder by using BrCH2CH2Br and SiMe3Cl and performing a reaction of the activated zinc powder and an organic halide to produce an organic zinc halide; and then performing a reaction of the organic zinc halide and a Grignard reagent of another halide to obtain the organic zinc compound. The organic zinc compounds with various structures can be produced by changing the groups on the organic halide.

Description

technical field [0001] The invention relates to a synthesis method of an organic zinc compound. Background technique [0002] Organozinc compounds are a class of organometallic compounds with wide application. Because organozinc compounds have good tolerance to functional groups, their halides are mostly used in the synthesis of organic compounds with multifunctional structures. It can also be used as an important reaction intermediate for the synthesis of optically active secondary alcohols (Chem. Rev. 1992, 92, 833; J. Am. Chem. Soc. 1999, 121, 3633). In recent years, organozinc compounds have been used as a "chain shuttling agent" in the field of olefin polymerization, which can creatively realize the controllable copolymerization of olefins and obtain new polymer materials (WO 2005 / 090427). [0003] For the synthesis of organozinc compounds with symmetrical structures, there have been many reports in the literature. The widely used method is to utilize the reaction of...

Claims

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Application Information

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IPC IPC(8): C07F3/06
Inventor 董金勇张传辉
Owner INST OF CHEM CHINESE ACAD OF SCI