Efficient synthesis method of compound of phenylpyridine tetrazacyclopentadiene (TAP)

A kind of technology of phenylpyridinetetrazapentylene and synthesis method, which is applied in the field of efficient synthesis of compound phenylpyridinetetrazapentylene, can solve problems such as TAP compound industrialized production is not formed, achieves process environmental protection and realizes industrialization , the effect of reducing production costs

Inactive Publication Date: 2019-01-15
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, with the exploitation of deep well oilfields in China, the demand for high-temperature heat-resistant explosives is also very urgent, and the industrial production of TAP compounds as intermediates has not yet formed.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 0.61g (0.0025mol) of BP raw material in 20mL of DMF, add 0.94g (0.0056mol) of triethyl phosphite raw material under magnetic stirring; raise the temperature to 130°C in an oil bath, continue the reaction for 6h, and complete the reaction; cool down When the temperature is lower than 30°C, it is poured into water to precipitate a solid, washed with water three times, filtered and dried to obtain phenylpyridine tetraazole with a yield of 81.5% and a purity of 96.8%.

Embodiment 2

[0020] Dissolve 0.61g of BP raw material in 20mL of DMF, add 0.94g of triethyl phosphite raw material under magnetic stirring; raise the temperature to 150°C in an oil bath, continue the reaction for 4h, and complete the reaction; cool down to below 30°C, pour into water The solid was precipitated, washed with water three times, filtered and dried to obtain the phenylpyridine tetraazolepentalcene with a yield of 83.8% and a purity of 97.2%.

Embodiment 3

[0022] Dissolve 0.61g of BP raw material in 20mL DMSO, add 0.94g of triethyl phosphite raw material under magnetic stirring; raise the temperature to 155°C in an oil bath, continue the reaction for 2h, and the reaction is complete; cool down to below 30°C, pour into water The solid was precipitated, washed with water three times, filtered and dried to obtain the phenylpyridine tetraazolepentalcene with a yield of 85.7% and a purity of 98.1%.

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PUM

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Abstract

The invention discloses an efficient synthesis method of a compound of phenylpyridine tetrazacyclopentadiene (TAP). 1-(3-nitryl-2-pyridine)-1H-benzotriazole (BP) is dissolved into a solvent; then, triethyl phosphite is added; reaction liquid reacts in a constant temperature bath; after the reaction is completed; the temperature of the reaction liquid is lowered to a value being 30 DEG C or below;the materials are poured into water; formed solid is filtered; water washing is performed for three times; after the dry filtering, drying is performed to obtain TAP. The synthesis method provided bythe invention has the advantages that the production period of a TAP compound can be shortened by four times or above; the production efficiency is improved; the industrial production of high-temperature heat-resistant explosives BPTAP can be favorably promoted; the production cost is reduced; the industrialization of the high-temperature heat-resistant explosives can be realized; meanwhile, the use of xylene toxic reagents is avoided; the process achieves the better environment-friendly effects.

Description

technical field [0001] The invention belongs to the category of organic compounds, more specifically, the invention relates to an efficient synthesis method of the compound phenylpyridine tetraazapentalene (TAP). Background technique [0002] Phenylpyridine tetraazapentalkene (TAP) is an important component of high-temperature heat-resistant explosive 2,4,8,10-tetranitro-phenylpyridine-1,3a,6,6a-tetraazapentalkalene (BPTAP). intermediate, and BPTAP is expected to be used in fields such as petroleum perforating bombs and high-energy heat-resistant explosives due to its good thermal stability. The synthesis of TAP was completed in foreign countries in the 1980s. The United States published the synthesis process of BPTAP in 2005, which included the synthesis process of TAP. It was refluxed in xylene solvent (143 ° C) for 24 hours, the reaction was completed, and the reaction time very long. There are no related reports in China. After repeated research, we found an efficient...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/14
CPCC07D471/14
Inventor 陈娅范桂娟马卿廖龙渝
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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