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Method for preparing octachloronaphthalene

A technology of chloronaphthalene and chlorine gas is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., and achieves the effects of mild production conditions, high yield and simple operation.

Inactive Publication Date: 2010-09-29
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] 1,2,3,4,5,6,7,8-octachloronaphthalene as shown in formula (II), be called for short octachloronaphthalene, be a kind of important chemical raw material, it has good chemical stability and Thermal stability, can be synthesized from naphthalene as a starting material, and there is no relevant report on its production technology

Method used

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  • Method for preparing octachloronaphthalene
  • Method for preparing octachloronaphthalene
  • Method for preparing octachloronaphthalene

Examples

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example 1

[0023] Add 128 grams of naphthalene, 0.56 grams of iron powder, and 700 grams of carbon tetrachloride into a 1000ML three-necked flask, stir to dissolve all the solids, and slowly raise the temperature. When the temperature of the reaction solution reaches 60°C, start feeding chlorine gas and 570 grams of chlorine gas, the tail gas was absorbed with 1N sodium carbonate aqueous solution, after 24 hours of reaction, the temperature was lowered, and when the temperature dropped to room temperature, it was filtered and dried to obtain 345 grams of crude product, which was dissolved in 1000 grams of toluene, heated to 60 °C, and added 15 grams of activated carbon were incubated for 15 minutes, filtered, the solution was cooled to room temperature, and the product was precipitated, filtered, and dried to obtain 310 grams of product with a yield of 76.8%, mp 192-194 ° C (the thermometer was not corrected), and a purity of 97.7%. . (HPLC method, mobile phase is methanol, flow velocity...

example 2

[0025] Add 128 grams of naphthalene, 0.65 grams of zinc powder, and 700 grams of tetrachlorethylene into a 1000ML three-necked flask, stir to dissolve all the solids, and slowly raise the temperature. When the temperature of the reaction solution reaches 90°C, start to feed chlorine gas. 640 grams, the tail gas was absorbed with 1N potassium carbonate aqueous solution, and after reacting for 16 hours, the temperature was lowered. After the temperature dropped to room temperature, it was filtered and dried to obtain 305 grams of crude product, which was dissolved with 800 grams of ethanol. After being heated to 50°C, add 15 Gac gac, insulation 15 minutes, filter, solution is cooled to room temperature, separate out product, filter, dry, obtain 278 grams, yield is 68.8%, mp 194-196 ℃ (the thermometer is not corrected), purity 98.5%.

example 3

[0027] Add 128 grams of naphthalene, 0.65 grams of zinc powder, and 700 grams of tetrachloroethane into a 1000ML three-necked flask, stir to dissolve all the solids, and slowly raise the temperature. 710 grams of chlorine gas, the tail gas was absorbed with saturated ammonia solution, after reacting for 6 hours, the temperature was lowered, and when the temperature dropped to room temperature, it was filtered and dried to obtain 305 grams of crude product, dissolved in 800 grams of acetone, heated to 40 ° C, added 15 Gram gac, insulation 15 minutes, filter, solution is cooled to room temperature, separate out product, filter, dry, obtain 246 grams, yield is 60.9%, mp 193-195 ℃ (the thermometer is not corrected), purity 98.3%.

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Abstract

The invention discloses a method for preparing octachloronaphthalene as shown in a formula (II). The method comprises the following steps: in an organic solvent, in the presence of a metal catalyst, controlling a temperature of naphthaline as shown in a formula (I) in the range of 60 to 130 DEG C; filling chlorine into the organic solvent to perform a reaction, wherein the amount of substance of the chlorine is 8.0 to 10.0 times that of naphthaline and the reaction time is in the range of 6 to 24 hours; and after the reaction is completed, processing reaction solution to obtain the octachloronaphthalene as shown in the formula (II), wherein the metal catalyst is ferrum or zinc and the organic solvent is carbon tetrachloride, tetrachloroethane or tetrachloroethylene. The raw materials adopted by the method are low-priced and are easily obtained. The method adopts the suitable organic solvent. And the organic solvent can be recycled. After the reaction, the processing is simple and the yield is high. The technical scheme of the invention has the advantages of mild production condition, safety and simple operation.

Description

(1) Technical field [0001] The present invention relates to a kind of preparation method of octachloronaphthalene. (2) Background technology [0002] 1,2,3,4,5,6,7,8-octachloronaphthalene as shown in formula (II), be called for short octachloronaphthalene, be a kind of important chemical raw material, it has good chemical stability and Thermal stability can be synthesized from naphthalene as a starting material, but there is no relevant report about its production technology at present. (3) Contents of the invention [0003] The object of the present invention is to provide a kind of preparation method of octachloronaphthalene. [0004] The technical scheme adopted in the present invention is: [0005] A preparation method of octachloronaphthalene as shown in formula (II), the method is: in an organic solvent, the naphthalene shown in formula (I), under the action of a metal catalyst, the temperature is controlled at 60 to 130°C , feed a sufficient amount of chlorine to...

Claims

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Application Information

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IPC IPC(8): C07C25/22C07C17/12
Inventor 潘建林黄敏沈华锋
Owner HANGZHOU NORMAL UNIVERSITY
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