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Production technique for preparing 5-alkyltetranitrozole by high pressure method

An alkane tetrazolium and production process technology, applied in the direction of organic chemistry and the like, can solve the problems of difficult pollution, low yield and high reaction temperature, and achieve the effect of less pollution

Inactive Publication Date: 2008-09-10
江苏德峰药业有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 5-alkane tetrazole is a very important medicine, pesticide and fine chemical intermediate, and its use is very extensive. In CN1995299, China Petrochemical Co., Ltd. applied 5-methyl tetrazole to cutting fluid composition Among them, it mainly solves the problem that cobalt is easy to seep out during the processing of cobalt-containing cemented carbide in the prior art
[0003] In the literature (1 Zhurnal Organiccheskoi Khimii, 24 (10), 2221-6; 1988; 2 DE3634717 1988) with acetonitrile, propionitrile as raw material with DMF as solvent, under the effect of aluminum trichloride and catalyst and azidation Synthesis of 5-methyltetrazolium and 5-ethyltetrazolium with sodium, not only the reaction temperature is high and the yield is low, but also because of the aluminum salt, the post-processing is difficult and the pollution is serious

Method used

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  • Production technique for preparing 5-alkyltetranitrozole by high pressure method
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  • Production technique for preparing 5-alkyltetranitrozole by high pressure method

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Experimental program
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Effect test

Embodiment 1

[0026] The feed ratio is acetonitrile: sodium azide: triethylamine hydrochloric acid: triethylamine=(molar ratio) 1:1:1.5:10.

[0027] After adding the reaction materials in the autoclave with stirring according to the above ratio, close the reactor, heat up to 130°C, and react for 8 hours. After the reaction, add liquid alkali to separate layers, and the oil layer is acidified to PH1-2 with hydrochloric acid. The water was distilled off under reduced pressure to obtain a solid product, and the distilled water was used to prepare liquid caustic soda with solid sodium hydroxide. The product solid was heated and extracted with ethyl acetate, and refined to obtain the product, with a content of 99.2% and a molar yield of 95.4%.

Embodiment 2

[0029] The feeding ratio is propionitrile: sodium azide: triethylamine hydrochloric acid: triethylamine=(molar ratio) 1:1:1.5:10.

[0030] After adding the reaction materials in the autoclave with stirring according to the above ratio, close the reactor, heat up to 130°C, and react for 8 hours. After the reaction, add liquid alkali to separate layers, and the oil layer is acidified to PH1-2 with hydrochloric acid. The water was distilled off under reduced pressure to obtain a solid product, and the distilled water was used to prepare liquid caustic soda with solid sodium hydroxide. The product solid was heated and extracted with ethyl acetate, and refined to obtain the product with a content of 99.4% and a molar yield of 93.2%.

Embodiment 3

[0032] The feed ratio is benzonitrile: sodium azide: triethylamine hydrochloric acid: triethylamine=(molar ratio) 1:1:1.5:10.

[0033] After adding the reaction materials in the autoclave with stirring according to the above ratio, close the reactor, heat up to 130°C, and react for 8 hours. After the reaction, add liquid alkali to separate layers, and the oil layer is acidified to PH1-2 with hydrochloric acid. The water was distilled off under reduced pressure to obtain a solid product, and the distilled water was used to prepare liquid caustic soda with solid sodium hydroxide. The product solid was heated and extracted with ethyl acetate, and refined to obtain the product with a content of 99.5% and a molar yield of 96.2%.

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Abstract

The invention discloses a production process using a high pressure method to prepare 5-alkane tetrazoline. Alkyl nitrile, sodium azide, triethylamine and triethylamine hydrochloric acid are mixed according to a certain proportion and then are plunged into a reaction kettle to react to generate 5-alkane tetrazoline; two reaction equations exist due to the difference of the raw material alkyl nitrile. The production process is easy to operate, and has high product yield, no waste water and small pollution.

Description

technical field [0001] The invention relates to a nitrogen-containing heterocyclic compound 5-alkane tetrazole and a preparation method thereof. Background technique [0002] 5-alkane tetrazole is a very important medicine, pesticide and fine chemical intermediate, and its use is very extensive. In CN1995299, China Petrochemical Co., Ltd. applied 5-methyl tetrazole to cutting fluid composition Among them, it mainly solves the problem that cobalt is easy to seep out during the processing of cobalt-containing cemented carbide in the prior art. The technical solution of the cutting fluid composition prepared from it and water etc. solves this problem well, and can be used in various cutting processes of cobalt-containing cutting tools or cobalt-containing materials to be processed. In addition, many patents of Fuji Corporation of Japan also use it in photosensitive materials. Many companies such as Dynamit Nobel Ag in Germany and Mitsubishi in Japan also use them in surface t...

Claims

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Application Information

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IPC IPC(8): C07D257/04
Inventor 王德峰朱小飞王炳才
Owner 江苏德峰药业有限公司
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