A method for one-step synthesis of 3,4-bis(4'-aminofurazan-3'-yl)oxyfurazan

A technology of aminofurazan and furoxan, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve problems such as high industrial production costs, large equipment footprint, and uncontrollable safety, and achieve Stable product quality, small footprint, good material mixing effect

Active Publication Date: 2022-05-03
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the existing methods of synthesizing DATF, there are many problems such as discharge of a large amount of waste water, complex operation process, uncontrollable safety, excessive equipment footprint, difficulty in industrial expansion, and high industrial production costs.

Method used

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  • A method for one-step synthesis of 3,4-bis(4'-aminofurazan-3'-yl)oxyfurazan
  • A method for one-step synthesis of 3,4-bis(4'-aminofurazan-3'-yl)oxyfurazan
  • A method for one-step synthesis of 3,4-bis(4'-aminofurazan-3'-yl)oxyfurazan

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Weigh 0.143 g (1.0 mmol, 1.0 equiv) of 3-amino-4-amidoxime furoxan (AAOF), add it to acetonitrile for dissolving, add 286 μL acetic acid (5.0 mmol, 5.0 equiv) to prepare a 4.5 mL solution, As material Ⅰ; weigh 0.069gNaNO 2 (1.0mmol, 1.0equiv) was added into water to prepare a 1.5mL solution as material Ⅱ. The feed pump simultaneously pumps in material I and material II, mixes them in the mixer, and transports them to a microchannel reactor (inner diameter 0.6mm, length 7m, volume 2mL) for reaction at a reaction temperature of 25°C. Among them, the flow rate of material I is 0.2mL / min, the flow rate of material II is 0.066mL / min, and the reaction residence time is 7.5min. The reaction effluent was collected and analyzed by high-performance liquid phase detection. The raw material conversion rate was 80.7%, and the product yield was 47.1%. figure 1 and figure 2 shown.

Embodiment 2

[0046]Weigh 0.143g (1.0mmol, 1.0equiv) of 3-amino-4-amidoxime furoxan (AAOF), add to acetonitrile to dissolve, add 278μL concentrated sulfuric acid (5.0mmol, 5.0equiv) to prepare a 4.5mL solution , as material Ⅰ; weigh 0.069gNaNO 2 (1.0mmol, 1.0equiv) was added into water to prepare a 1.5mL solution as material Ⅱ. The feed pump simultaneously pumps in material I and material II, mixes them in the mixer, and transports them to a microchannel reactor (inner diameter 0.6mm, length 7m, volume 2mL) for reaction at a reaction temperature of 25°C. Among them, the flow rate of material I is 0.2mL / min, the flow rate of material II is 0.066mL / min, and the reaction residence time is 7.5min. The reaction effluent was collected and analyzed by high performance liquid phase detection. The conversion rate of the raw material was 86.7%, and the yield of the product was 54.1%.

Embodiment 3

[0048] Weigh 0.143g (1.0mmol, 1.0equiv) of 3-amino-4-amidoxime furoxan (AAOF), add to acetonitrile to dissolve, add 333μL concentrated nitric acid (5.0mmol, 5.0equiv) to prepare a 4.5mL solution , as material Ⅰ; weigh 0.069gNaNO 2 (1.0mmol, 1.0equiv) was added into water to prepare a 1.5mL solution as material Ⅱ. The feed pump simultaneously pumps in material I and material II, mixes them in the mixer, and transports them to a microchannel reactor (inner diameter 0.6mm, length 7m, volume 2mL) for reaction at a reaction temperature of 25°C. Among them, the flow rate of material I is 0.2mL / min, the flow rate of material II is 0.066mL / min, and the reaction residence time is 7.5min. The reaction effluent was collected and analyzed by high performance liquid phase detection. The conversion rate of the raw material was 82.6%, and the yield of the product was 50.3%.

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Abstract

The invention belongs to the field of chemical synthesis, and specifically discloses a method for synthesizing 3,4-bis(4'-aminofurazan-3'-yl)furazan oxide in one step using a microchannel reactor. ‑Amidoxime furazan solution and sodium nitrite aqueous solution are simultaneously pumped into the micro-mixer of the microchannel reactor, and after mixing, they are passed into the microreactor for reaction to obtain 3,4-bis(4'-aminofurazan -3'-yl) reaction solution of furazan oxide. The reaction process of the invention realizes one-step direct synthesis from the raw material AAOF to the target product DATF, has the advantages of short reaction time, high conversion rate of raw materials, high yield of target product, etc., and has good industrial application prospects.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for synthesizing 3,4-bis(4'-aminofurazan-3'-yl)furazan by one-step method using a microchannel reactor. Background technique [0002] Furazan compounds are important types of high-energy-density compounds and high-nitrogen-containing compounds, which have the advantages of high energy density, stew, and high nitrogen content. Furazan ring is a five-membered ring planar structure containing 2 carbon atoms, 2 nitrogen atoms and 1 oxygen atom, and the molecular formula is C 2 N 2 Oh 2 , also known as oxadiazole ring, its nitrogen content is 37%, carbon content is 34%, oxygen content is 23%, and six electrons on the ring form a conjugated large π bond, which has a certain aromaticity. Its energy source is based on the large number of carbon-nitrogen and nitrogen-nitrogen bonds in the molecule; for the design of high-energy-density compounds containing C, H, O...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D271/08B01J19/00
CPCC07D271/08B01J19/0093
Inventor 郭凯覃龙州邱江凯袁鑫孙蕲段秀
Owner NANJING TECH UNIV
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