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Method for synthesizing tetracyclo[7.3.1.02,7.17,11]tetradecane

A synthetic method, tetradecane technology, applied in the direction of isomerization hydrocarbon production, organic chemistry, etc., can solve the problems of complex product separation and low yield, and achieve high reaction yield, high reaction yield and simple process Effect

Active Publication Date: 2010-07-21
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction product of this method needs to be separated from the solvent by distillation, and a large amount of acidic waste water is produced in the post-treatment process of catalysts such as aluminum halide, ferric chloride or sulfuric acid, and the product separation is complicated and the yield is low.

Method used

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  • Method for synthesizing tetracyclo[7.3.1.02,7.17,11]tetradecane

Examples

Experimental program
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Effect test

preparation example Construction

[0019] Preparation of chloroaluminate ionic liquid:

[0020] Add a certain amount of alkylamine chloride, alkylimidazole halide or alkylpyridine halide into a one-mouth bottle with magnetic stirring, stir, heat up to 60°C, add anhydrous aluminum trichloride in a certain molar ratio, and pump Vacuum for 1h to prepare the corresponding chloroaluminate ionic liquid.

Embodiment 1

[0022] Add 0.1mol methylamine bromide-aluminum trichloride ionic liquid to a three-necked flask equipped with a thermometer and mechanical stirring, the mol ratio of aluminum trichloride to methylamine bromide in the ionic liquid is 0.75:1, stir Add 0.1mol tetracycline [7.4.0.0 2，7 .1 3，6 ]Tetradecane, reacted at 50°C for 4h, cooled after the reaction, left to stand, separated, the ionic liquid in the lower layer was recovered and used, and the colorless transparent liquid in the upper layer was the product tetracycline [7.3.1.0 2，7 .1 7，11 ] Tetradecane, gas chromatography analysis, yield 98%.

[0023] Product structure identification:

[0024] MS: m / z 190 (M + ), 121(100).

[0025] IR(KBr), υ / cm -1 : 2905, 2848, 1449, 1346, 1097.

[0026] 13 CNMR (CDCl 3 ), δ / ppm: 23.92 (CH 2 , C5), 26.40 (CH 2 , C3), 26.71 (CH 2 , C4), 29.34 (CH, C9, C11), 31.3 (CH, C1, C7), 35.90 (CH 2 , C12, C13), 38.11 (CH 2 , C10), 38.72 (CH 2 , C6), 40.41 (CH, C2), 40.43 (CH 2 , C14), 4...

Embodiment 2

[0029] Add 0.2mol butylpyridine iodide-aluminum trichloride ionic liquid in the there-necked flask equipped with thermometer and mechanical stirring, the aluminum trichloride of this ionic liquid and iodide butylpyridine mol ratio are 0.5: 1, under stirring Add 0.1mol tetracycline [7.4.0.0 2，7 .1 3，6 ] Tetradecane, react at 70°C for 6h, cool after the reaction, let stand, separate the liquid, recycle the ionic liquid in the lower layer, and use the colorless transparent liquid in the upper layer as the product tetracycline [7.3.1.0 2，7 .1 7，11 ] Tetradecane, gas chromatography analysis, yield 97.8%.

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Abstract

The invention discloses a method for synthesizing tetracyclo[7.3.1.02,7.17,11]tetradecane and aims to solve the problems of a large amount of acidic wastewater, complex product separation and low yield of the prior art. In the method, tetracyclo[7.4.0.02,7.13,6]tetradecane serving as a raw material reacts in the presence of chloroaluminate ionic liquid at 50 to 130 DEG C for 1 to 8 hours; the product is cooled and stood for layering to obtain the tetracyclo[7.3.1.02,7.17,11]tetradecane, wherein the molar ratio of the chloroaluminate ionic liquid to the tetracyclo[7.4.0.02,7.13,6]tetradecane is 0,05-2:1; the chloroaluminate ionic liquid may be chloroalkylamine-aluminium choride, haloalkylimidazole-aluminium choride or haloalkylpyridine- aluminium choride; and the molar ratio of the aluminium choride to the haloalkylamine, haloalkylimidazole or the haloalkylpyridine is 0.5-1:1. The method is mainly used for synthesizing tetracyclo[7.3.1.02,7.17,11]tetradecane hydrocarbon fuel.

Description

technical field [0001] The present invention relates to a tetracyclic [7.3.1.0 2，7 .1 7，11 ] The synthetic method of tetradecane belongs to organic synthesis. Background technique [0002] Four Rings [7.3.1.0 2，7 .1 7，11 ]Tetradecane is an important fine chemical and a hydrocarbon fuel with excellent performance, mainly used as ramjet fuel or fuel component. [0003] Currently, four rings [7.3.1.0 2，7 .1 7，11 ] Tetradecane's synthetic method is in the presence of organic solvent and acidic catalyst, tetracycline [7.4.0.0 2，7 .1 3，6 ] tetradecane isomerization reaction prepared. For example US 4762092 discloses a tetracyclic [7.3.1.0 2，7 .1 7，11 ] the synthetic method of tetradecane, this method is catalyst with Lewis acid such as aluminum halide, ferric chloride or sulfuric acid, in aliphatic saturated hydrocarbon or halogenated hydrocarbon solvent, synthetic tetracyclic [7.3.1.0 2，7 .1 7，11 ] Tetradecane, the reaction yield is 92.8%. However, the reaction produ...

Claims

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Application Information

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IPC IPC(8): C07C13/68C07C5/29
Inventor 吕剑杜咏梅李春迎亢建平张伟曾纪珺寇联岗刘波
Owner XIAN MODERN CHEM RES INST
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