Synthesis method of 3,4-bi(4'-nitrophenyl) oxidized furoxan

Abstract

The invention discloses a synthesis method of 3,4-bi(4'-nitrophenyl) oxidized furoxan. The structure formula thereof is shown as (I), and the synthesis method adopts p-nitrobenzaldehyde as raw material; the structure formula thereof is shown as (II), and the synthesis method comprises the following steps: 1) adding the p-nitrobenzaldehyde and alcohol into a reaction flask, then adding hydroxylamine hydrochloride aqueous solution, using Na2CO3 aqueous solution to adjust pH of reaction liquid to 6 to 8, reacting for 1 to 2 hours at the temperature of 10 to 40 DEG C, obtaining p-nitrobenzaldoxime, with the molar ratio of the p-nitrobenzaldehyde and hydroxylamine hydrochloride of 1:1 to 1:1.5; and 2) adding the p-nitrobenzaldoxime, chlorosuccinimide and trichloromethane into the reaction flask, with the molar ratio of the p-nitrobenzaldoxime and chlorosuccinimide of 1:1 to 1:1.5, reacting for 1 to 3 hours at the temperature of 20 to 40 DEG C, using Na2CO3 solution to adjust pH of a system to 6 to 8 at the temperature of 0 to 5 DEG C, reacting for 1 to 4 hours and obtaining the objective product, namely the 3,4-bi(4'-nitrophenyl) oxidized furoxan. The synthesis method is mainly used for the 3,4-bi(4'-nitrophenyl) oxidized furoxan.

Description

technical field The invention relates to a synthesis method of 3,4-bis(4'-nitrophenyl)furazan. Background technique Furazan oxides are an important class of energetic compounds. Furazan oxide rings in the molecule as explosive groups can provide relatively higher energy density; furazan oxide derivatives can improve the oxygen balance of the system as energetic additives. Increase the detonation pressure; In addition, the furoxan ring can also endow its derivatives with ring tension and high standard enthalpy of formation. 3,-bis(4'-nitrophenyl)furoxan is an energetic material with good thermal stability and high energy density. The main synthesis method of 3,4-bis(4'-nitrophenyl)furoxan is dimerization of nitrile oxide. For example, "Synthesis and characterization of diarylfuroxans" (Defence Science Journal, 2006, 56, 4, 551-557) discloses a synthetic method of 3,4-bis(4'-nitrophenyl)furoxans, which uses p-Nitrobenzaldehyde is a raw material, and its synthetic route is ...

AI Technical Summary

Problems solved by technology

But the intermediate p-nitrobenzoyl chloride oxime of this method can carry out next step reaction after extracting and separating, and reaction steps is more and reaction cycle is longer

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