Method for synthesizing pentacyclo[6.3.1.0(2,7).0(3,5).0(9,11)]dodecane

A synthesis method and technology of dodecane, applied in the direction of condensation between hydrocarbons and non-hydrocarbons to produce hydrocarbons, organic chemistry, etc., can solve the problems of easy water absorption and decomposition, loss of catalytic activity, etc., and achieve the effect of easy preparation

Active Publication Date: 2008-08-13
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Catalyst cuprous chloride in the method is easily oxidized to cupric chloride in air, loses catalytic activity; Taiwan patent 118607 also discloses another kind with dicyclopentadiene and diiodomethane as raw material, triethylaluminum as The catalyst obtained the pentacyclic [6.3.1.0 2，7 .0 3，5 .0 9，11 ] Pentacyclo of dodecan

Method used

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  • Method for synthesizing pentacyclo[6.3.1.0(2,7).0(3,5).0(9,11)]dodecane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of catalyst zinc-copper alkaloid:

[0026] Add 100mL of 3.5% HCl to 100g of zinc powder, stir for 2min and then filter, then add 100mL of water to the zinc powder, stir for 2min, filter, repeat the washing process three times. Add 100mL of 2% CuSO to the washed zinc powder 4 The aqueous solution was stirred for 5 minutes, and filtered to obtain the catalyst zinc-copper alkaloid.

[0027] Five rings [6.3.1.0 2，7 .0 3，5 .0 9，11 ] Preparation of dodecane

[0028] Place the reaction bottle with mechanical stirring, thermometer, and reflux condensing device in the ultrasonic reactor, add 0.4mol zinc copper alkene, 0.1mol dicyclopentadiene, 0.4mol CH 2 I 2 and 0.2mol ether were added to the reaction flask, then under stirring, 0.02mol I was added 2 ; Turn on the ultrasonic reactor, heat up, the reaction temperature rises to 40°C, react for 3 hours, stop the reaction and cool down to room temperature naturally; filter the reaction solution, remove the cataly...

Embodiment 2

[0037] Place the reaction bottle with mechanical stirring, thermometer, and reflux condensing device in the ultrasonic reactor, add 0.8mol zinc copper alkene, 0.1mol dicyclopentadiene, 0.8mol CH 2 I 2 and 0.4mol dioxane are added to the reaction flask, then under stirring, add 0.04mol I 2 ; Turn on the ultrasonic reactor, heat up, the reaction temperature rises to 50°C, react for 0.5h, stop the reaction and cool to room temperature naturally; filter the reaction solution, remove the catalyst, distill the filtrate under reduced pressure, and collect at 115°C to 118°C under a vacuum of 5KPa Distillate to get the product.

[0038] Through gas chromatography analysis, the conversion rate of this example is 99.3%, and the yield is 95.1%.

Embodiment 3

[0040] Place the reaction bottle with mechanical stirring, thermometer, and reflux condensing device in the ultrasonic reactor, add 0.7mol zinc copper alkene, 0.1mol dicyclopentadiene, 0.7mol CH 2 I 2 and 0.35mol dioxane are added to the reaction flask, then under stirring, add 0.035mol I 2 ; Turn on the ultrasonic reactor, heat up, the reaction temperature rises to 40°C, react for 1h, stop the reaction and cool down to room temperature naturally; filter the reaction solution, remove the catalyst, distill the filtrate under reduced pressure, and collect fractions at 115°C to 118°C under a vacuum of 5KPa , get the product.

[0041] Through gas chromatography analysis, the conversion rate of this example is 99.7%, and the yield is 95.3%.

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Abstract

The invention discloses a synthesis method of pentacyclic [6.3.1.0<2, 7>.0<3, 5>.0<9,11>] dodecane to solve the problem of low yield. The invention uses dicyclopentadiene and diiodomethane as materials, comprises following steps of: (1) setting a reaction bottle in an ultrasonic reactor, adding and mixing zinc copper alloy, dicyclopentadiene, diiodomethane, iodine and ethers organic solvent; (2) starting the ultrasonic reactor, in which the reaction temperature is 30 DEG C - 50 DEG C, the reaction time is 0.5h-5h; (3) filtering the reaction liquid, removing the catalyst, decompressing the distillation filtering liquid so as to obtain pentacyclic [6.3.1.0<2, 7>.0<3, 5>.0<9, 11>] dodecane. The invention is short in reaction time, high in yield, and is mainly used in synthesis of pentacyclic [6.3.1.0<2, 7>.0<3, 5>.0<9, 11>] dodecane.

Description

technical field [0001] The present invention relates to a pentacyclic [6.3.1.0 2，7 .0 3，5 .0 9，11 ] The synthesis method of dodecane belongs to organic synthesis. Background technique [0002] Five rings [6.3.1.0 2，7 .0 3，5 .0 9，11 ] Dodecane, commonly known as dicyclopentadiene cyclopropane compound, density greater than 1.0g / cm 3 , the heat of combustion is greater than 44MJ / L, and it is usually in a liquid state. It has the characteristics of low freezing point, high density, and high heat of combustion. It can be used as fuel for racing cars, rowing boats, etc., and can also be used as missile fuel. [0003] Currently known five rings [6.3.1.0 2，7 .0 3，5 .0 9，11 ] In the synthetic method of dodecane, Taiwan patent 118607 discloses to take dicyclopentadiene and methylene bromide as raw materials, zinc powder and cuprous chloride as catalyst, obtain pentacyclic [6.3.1.0 2，7 .0 3，5 .0 9，11 ] Pentacyclo of dodecane [6.3.1.0 2，7 .0 3，5 .0 9，11 ] The synthetic m...

Claims

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Application Information

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IPC IPC(8): C07C13/62C07C2/86
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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