Efficient synthesis method of 1-(3-nitry-2-pyridine)-1H-benzotriazole compound

A technology of benzotriazole and synthesis method, which is applied in the field of efficient synthesis of 1--1H-benzotriazole compounds, can solve problems such as the unformed industrial production of BP compounds, shorten the production cycle, reduce production costs, and improve The effect of production efficiency

Inactive Publication Date: 2018-02-16
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 development of deep well oilfields in China, the demand for high-temperature heat-resistant explosives is also very urgent, and the industrial production of BP compounds as intermediates has not yet formed.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Dissolve 0.1181g of benzotriazole raw material in 10mL of DMF, add 0.1561g of 2-chloro-3-nitropyridine raw material under magnetic stirring, then add 0.1073g of anhydrous calcium carbonate; heat up to 80°C in a water bath, The reaction continued for 45 minutes, and the reaction was all completed; the temperature was lowered to below 30°C, and the precipitate was precipitated in water, filtered and dried.

Embodiment 2

[0024] Dissolve 0.1185 g of benzotriazole raw material in 10 mL of DMF, add 0.1567 g of 2-chloro-3-nitropyridine raw material under magnetic stirring, and then add 0.1078 g of anhydrous calcium carbonate; heat up to 40 ° C in a water bath, The reaction was continued for 8 hours, and the reaction was all completed; the temperature was lowered to below 30°C, and the precipitate was precipitated in water, filtered and dried.

Embodiment 3

[0026] Dissolve 0.1786g of benzotriazole raw material in 10mLDMSO, add 0.2355g of 2-chloro-3-nitropyridine raw material under magnetic stirring, then add 0.1596g of anhydrous calcium carbonate; heat up to 80°C in a water bath, The reaction was continued for 20 minutes, and the reaction was all completed; the temperature was lowered to below 30°C, and the precipitate was precipitated in water, filtered and dried.

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Abstract

The invention discloses an efficient synthesis method of a 1-(3-nitry-2-pyridine)-1H-benzotriazole compound. The synthesis method comprises the following steps: (1) weighing a certain solvent, addinga certain amount of benzotriazole raw material under the stirring state, adding a 2-chlorine-3-nitropyridine raw material with molar weight equal to that of the benzotriazole raw material, finally adding a certain amount of anhydrous sodium carbonate to form reaction liquid and maintaining the stirring state; (2) putting the reaction liquid into constant-temperature bath, continuously maintainingthe stirring state, and reacting at a certain temperature; and (3) after the reaction, cooling the reaction liquid to be below 30 DEG C, pouring into water, filtering and drying to obtain the 1-(3-nitry-2-pyridine)-1H-benzotriazole (BP) compound. By the synthesis method, the production cycle of the BP compound can be shortened by 3 to 12 times, the production efficiency is improved, the industrialized production of BPTAP can be promoted, the production cost can be reduced, and industrialization of high-temperature heat-resistant explosive is realized.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a highly efficient synthesis method of 1-(3-nitro-2-pyridine)-1H-benzotriazole (BP) compound. Background technique [0002] 1-(3-nitro-2-pyridine)-1H-benzotriazole (BP) is a high-temperature heat-resistant explosive 2,4,8,10-tetranitro-phenylpyridine-1,3a,6,6a- An important intermediate of tetraazapentalpine (BPTAP), 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 BP and its derivatives has been completed in foreign countries in the 1980s. The United States published the synthesis process of BPTAP in 2005, which includes the synthesis process of BP. The reaction needs to be carried out for 24 hours under the reflux of acetonitrile (boiling point: 81.6 ° C), and the reaction time is very long. The researchers of the Xi'an Institute of Modern Chemistry in Chin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 陈娅屈延阳范桂娟程碧波
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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