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Method for synthesizing hanger-type-tricycl [5.2.1.02,6] decane

A synthesis method and technology of decane, applied in the direction of isomerization hydrocarbon production, organic chemistry, etc., can solve the problems of high reaction conversion rate, less by-products, difficult separation, etc., and achieve simple product separation, high conversion rate and yield , The effect of constant catalytic activity

Active Publication Date: 2007-12-05
XIAN MODERN CHEM RES INST
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AI Technical Summary

Problems solved by technology

Wherein the chloroaluminate ionic liquid has certain acidity, the chloroaluminate ionic liquid that aluminum trichloride and halogenated alkylimidazole or halogenated alkylpyridine make are used for hanging-tricyclic [5.2.1.0 2，6 ] The synthesis of decane not only plays the role of catalyst but also plays the role of solvent, the reaction conversion rate is high, the by-product is few, and the separation of product and ionic liquid can be realized by adopting the liquid separation method, which solves the separation difficulty of the prior art The problem

Method used

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  • Method for synthesizing hanger-type-tricycl [5.2.1.02,6] decane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Preparation of chloroaluminate ionic liquid:

[0022] Add 1 part of molar mass of ethylpyridine iodide to the reaction flask, stir, heat up to 85°C, add 1.8 parts of molar mass of anhydrous aluminum trichloride, stir, and vacuumize for 1 hour to obtain ethylpyridine iodide-tri Aluminum chloride ionic liquid.

[0023] Add 0.1 mol of ethylpyridine iodide-aluminum trichloride ionic liquid to a flask equipped with a thermometer and stirring, and add 0.2 mol of bridge-tricyclic [5.2.1.0 2，6 ] decane, reacted at room temperature for 2h, cooled after the reaction, left standstill, the lower layer of ionic liquid was recovered for use, and the upper layer of colorless transparent liquid was the product hanging type-tricyclic [5.2.1.0 2，6 ] Decane, analyzed by gas chromatography, the reaction conversion rate was 99.7%, and the yield was 99.3%.

[0024] Product structure identification:

[0025] MS: m / z 136 (M + ), 67(100).

[0026] IR(KBr), υ / cm -1 : 2946, 2866, 1468, 1456...

Embodiment 2

[0030] Preparation of chloroaluminate ionic liquid:

[0031] The preparation method of the ionic liquid is the same as in Example 1, except that the raw materials are 1-methyl-3-ethylimidazole bromide and aluminum trichloride, and the molar ratio is 1.5.

[0032] Add 0.075 mol of 1-methyl-3-ethylimidazole bromide-aluminum trichloride ionic liquid into a flask equipped with a thermometer and stirring, and add 0.1 mol of bridge-tricyclic [5.2.1.0 2，6 ] decane, control the reaction temperature to 45°C, react for 1.5h, cool down after the reaction, let it stand, the lower layer of ionic liquid is recycled, and the upper layer of colorless transparent liquid is the product hanging type-tricyclic [5.2.1.0 2，6 ] Decane, analyzed by gas chromatography, the reaction conversion rate was 99.5%, and the yield was 98.9%.

Embodiment 3

[0034] Preparation of chloroaluminate ionic liquid:

[0035] The preparation method of the ionic liquid is the same as in Example 1, except that the raw materials are butylpyridine chloride and aluminum chloride, and the molar ratio is 1.55.

[0036] Add 0.1mol butylpyridine chloride-aluminum trichloride ionic liquid to a flask equipped with a thermometer and stirring, and add 0.1mol bridge-tricyclic [5.2.1.0 2，6 ] decane, control the reaction temperature to 100°C, react for 20min, cool down after the reaction, let it stand, the lower layer of ionic liquid is recycled and used, and the upper layer of colorless transparent liquid is the product hanging type-tricyclic [5.2.1.0 2，6 ] Decane, analyzed by gas chromatography, the reaction conversion rate was 99.0%, and the yield was 98.3%.

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Abstract

The present invention discloses process of synthesizing exo-tricyclo[5.2.1.02, 6] decane, and aims at solving the technological problem of raising reaction conversion rate and yield and separating product from by product effectively. The process includes the following steps: adding chloroaluminic acid ionic liquid in a reactor, adding bridge-tricyclo[5.2.1.02, 6] decane material to react at 5-100 deg.c for 20 min to 2 hr, letting the reactant liquid stand and separating exo-tricyclo[5.2.1.02, 6] decane. The molar ratio between the chloroaluminic acid ionic liquid and bridge-tricyclo[5.2.1.02, 6] decane is 0.5-5, and the chloroaluminic acid ionic liquid is alkyl imidazole halide-aluminum trichloride or alkyl pyridine halide-aluminum trichloride. The present invention is applied mainly in synthesizing exo-tricyclo[5.2.1.02, 6] decane.

Description

technical field [0001] The present invention relates to a hanging type-tricyclic [5.2.1.0 2，6 ] The synthesis method of decane belongs to organic synthesis. Background technique [0002] Hanging-Three Rings [5.2.1.0 2，6 ]Decane, commonly known as hanging tetrahydrodicyclopentadiene (exo-THDCPD), is an important fine chemical intermediate, mainly used for the synthesis of adamantane, and also a hydrocarbon fuel with excellent performance, which can be used as a fuel group point. [0003] Hanging-Three Rings [5.2.1.0 2，6 The synthesis of decane is mostly through bridge-tricyclo[5.2.1.0 2，6 ] The isomerization reaction of decane is realized, and the known hanging type-tricyclo[5.2.1.0 2，6 ] In the decane synthesis method, the catalysts used are mostly acidic catalysts and organic solvents are used. US 3381046 discloses the suspension-tricyclic [5.2.1.0 2，6 ] the synthetic method of decane, produces a large amount of spent acid in the processing process, to reaction conve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/61C07C5/22
Inventor 吕剑李春迎杜咏梅谷玉杰李凤仙亢建平
Owner XIAN MODERN CHEM RES INST
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