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(Z)-1, 4, 7, 10-tetraoxocyclododecane-8-alkene lithium salt complex, preparation method and application thereof

A technology of tetraoxcyclododecane and tetraoxahexadecane is applied in the field of synthesizing crown ether compounds, which can solve the problems of difficult product purification, high risk of raw materials, low product yield, etc. The effect of labor cost, high reaction selectivity and high product yield

Active Publication Date: 2021-08-06
河北百灵威超精细材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] The purpose of the present invention is to provide a kind of (Z)-1,4,7,10-tetraoxocyclododecane-8-ene lithium salt complex, preparation method and application thereof, for solving the problems in the prior art There are technical problems such as poor safety, high risk of raw materials, difficult product purification and low product yield in the preparation of lithium ion carrier V

Method used

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  • (Z)-1, 4, 7, 10-tetraoxocyclododecane-8-alkene lithium salt complex, preparation method and application thereof
  • (Z)-1, 4, 7, 10-tetraoxocyclododecane-8-alkene lithium salt complex, preparation method and application thereof
  • (Z)-1, 4, 7, 10-tetraoxocyclododecane-8-alkene lithium salt complex, preparation method and application thereof

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preparation example Construction

[0052] The present invention also provides a preparation method of (Z)-1,4,7,10-tetraoxocyclododecane-8-ene lithium salt complex, which comprises the following steps:

[0053]

[0054] Using compound R as a raw material, react with compound lithium salt LiX in the first reaction solvent, under the catalysis of ring-closing metathesis reaction catalyst and the protection of inert gas, under the condition of temperature range of -20 ~ 150 ℃, the reaction is complete The compound (Z)-1,4,7,10-tetraoxocyclododecane-8-ene lithium salt complex was obtained;

[0055] Wherein, R is selected from (2E,14E)-4,7,10,13-tetraoxahexadecane-2,14-diene, 3,6,9,12-tetraoxatetradecane-1, 13-diene, (2Z,14Z)-4,7,10,13-tetraoxahexadecane-2,14-diene, 4,7,10,13-tetraoxahexadecane-2, 14-diene, 5,8,11,14-tetraoxaoctadecane-3,15-diene, (3E,15E)-5,8,11,14-tetraoxaoctadecane-3, 15-diene, (3Z,15Z)-5,8,11,14-tetraoxaoctadecane-3,15-diene;

[0056] X is selected from fluorine, chlorine, bromine, iodine,...

Embodiment 1

[0076]

[0077] Step (a): Preparation of formula 3 compound (Z)-1,4,7,10-tetraoxocyclododecane-8-ene lithium chloride complex

[0078] Maintaining a slight positive pressure of nitrogen, add 60L ethyl acetate and 1.28kg formula 2 compound lithium chloride to the 100L reaction kettle successively, stir well; then add 1g GRELA2 generation catalyst to it, stir well; Add 6.91kg of the compound of formula 1 (2E,14E)-4,7,10,13-tetraoxahexadecane-2,14-diene dropwise into the reaction solution, control the rate of addition, drop it in 3 hours, stir well, The gas generated during the reaction is introduced into the potassium permanganate aqueous solution, which will produce olefin gas, but the danger is much lower than hydrogen gas, which can be absorbed by the potassium permanganate aqueous solution, while the hydrogen gas produced by the prior art cannot be absorbed . When the color of the potassium permanganate aqueous solution starts to lighten, it is necessary to add potassium...

Embodiment 2

[0093]

[0094] Step (a): Preparation of formula 3 compound (Z)-1,4,7,10-tetraoxocyclododecane-8-ene lithium chloride complex

[0095] Maintaining a slight positive pressure of nitrogen, sequentially add 60L of ethyl acetate and 1.28kg of formula 2 compound lithium chloride into the 100L reactor, and stir well; then add 1g of GRELA 2nd generation catalyst to it, stir well; the temperature of the reaction solution is raised to 50°C, Add 6.07kg formula 1 compound 3,6,9,12-tetraoxatetradecane-1,13-diene dropwise in the reaction solution, control the rate of addition, drop it in 3 hours, stir well, the The gas is introduced into the potassium permanganate aqueous solution, and when the color of the potassium permanganate aqueous solution starts to become lighter, potassium permanganate needs to be added thereto. The reaction solution was kept at 50° C. to continue the reaction for 8 hours, and the reaction was completed.

[0096] The reaction solution was naturally cooled to r...

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Abstract

The invention discloses a (Z)-1, 4, 7, 10-tetraoxocyclododecane-8-alkene lithium salt complex as well as a preparation method and application thereof. The chemical structure of the (Z)-1, 4, 7, 10-tetraoxocyclododecane-8-alkene lithium salt complex is shown in the specification, and X is selected from fluorine, chlorine, bromine, iodine, p-toluenesulfonyl oxygen, methylsulfonyl oxygen, boron tetrafluoride, phosphorus hexafluoride, p-nitrobenzenesulfonyl oxygen and o-nitrobenzenesulfonyl oxygen. The method has the advantages of reasonable route design, safe and easily available raw materials, high process safety, high reaction selectivity, simple purification, high product purity and high product yield, and can fully meet the requirements of industrial production of products.

Description

technical field [0001] The invention relates to the technical field of synthesis of crown ether compounds, in particular to a (Z)-1,4,7,10-tetraoxocyclododecane-8-ene lithium salt complex and a preparation method thereof, and the use of Method for preparing lithium ion carrier V from this complex. Background technique [0002] Crown ether, also known as "crown compound", is a special class of macrocyclic polyether, named for its three-dimensional shape resembling a crown. The hole structure of crown ether has a good selection effect on ions because of its special size. Lithium ion carrier V (chemical name 12-crown ether-4, CAS 294-93-9) is a kind of crown ether, the size of its hole structure is equivalent to the size of lithium ions, and it is a very good choice for lithium ions capacity for sexual bonding. According to the latest literature report (J.Am.Chem.Soc., 2020, 142, 21082-21090), the artificial ion transmembrane transporter prepared by linking lithium ion carri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D323/00
CPCC07D323/00
Inventor 龙韬刘文彬
Owner 河北百灵威超精细材料有限公司
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