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Method for synthesizing 3, 4-di (fluorine geminal dinitro) dinitrofurzananofuroxan

A technology of fluoro-gem-dinitro and furoxan, which is applied in the field of synthesis of 3,4-dioxyfurazan, can solve the problems of cumbersome processing and low yield, and achieve the effect of simple post-processing

Inactive Publication Date: 2016-08-17
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

But this method yield is low, only 10%; This method is loaded down with trivial details simultaneously, needs n-hexane and methylene dichloride secondary extraction, also needs to separate with column chromatography then

Method used

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  • Method for synthesizing 3, 4-di (fluorine geminal dinitro) dinitrofurzananofuroxan
  • Method for synthesizing 3, 4-di (fluorine geminal dinitro) dinitrofurzananofuroxan
  • Method for synthesizing 3, 4-di (fluorine geminal dinitro) dinitrofurzananofuroxan

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Embodiment 1

[0018] Under stirring, add 0.74g (2mmol) of 3,4-bis(dinitromethyl)furazan dipotassium salt into 15mL of acetonitrile, then add 2.03g (12mmol) of xenon difluoride, and react at a temperature of 25°C 96h, concentrate the reaction solution, pour the obtained concentrated solution into water, use dichloromethane (10mL×3) to extract the reaction solution, combine the extracts, wash with water, dry, and distill under reduced pressure to obtain a colorless oily liquid 3,4- Bis(fluoro-gem-dinitro)furoxan 0.39g, yield 59.0%, purity 98.6%;

[0019] Structure Identification:

[0020] Infrared Spectrum: IR(KBr,cm -1 )ν: 1662, 1611, 1484, 1360, 1342, 1300, 1260, 1212, 1158, 989, 926, 835, 793, 705, 632;

[0021] NMR spectrum: 13 CNMR (CDCl 3 ,125MHz), δ:141.70,114.62,113.91,103.84; 19 F NMR (DMSO-d 6 ,470.5MHz), δ:-93.87,-100.16;

[0022] Elemental Analysis: Structural Formula C 4 N 6 o 10 f 2

[0023] Theoretical value: C 14.56, N 25.46

[0024] Measured value: C 14.48, N 25....

Embodiment 2

[0027] Under stirring, add 0.74g (2mmol) of 3,4-bis(dinitromethyl)furazan dipotassium salt into 15mL of acetonitrile, then add 2.03g (12mmol) of xenon difluoride, and react at a temperature of 20°C 100h, concentrate the reaction solution, pour the obtained concentrated solution into water, extract the reaction solution with dichloromethane (10mL×3), combine the extracts, wash with water, dry, and distill under reduced pressure to obtain a colorless oily liquid 3,4- Bis(fluoro-gem-dinitro)furoxan 0.34 g, yield 51.4%, purity 98.5%.

Embodiment 3

[0029] Under stirring, add 0.74g (2mmol) of 3,4-bis(dinitromethyl)furazan dipotassium salt into 15mL of acetonitrile, then add 2.03g (12mmol) of xenon difluoride, and react at a temperature of 15°C 80h, concentrate the reaction solution, pour the obtained concentrated solution into water, extract the reaction solution with dichloromethane (10mL×3), combine the extracts, wash with water, dry, and distill under reduced pressure to obtain a colorless oily liquid 3,4- Bis(fluorogem-dinitro)furoxan 0.22 g, yield 33.0%, purity 97.3%.

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Abstract

The invention discloses a method for synthesizing 3, 4-di (fluorine geminal dinitro) dinitrofurzananofuroxan. The method includes steps of adding 3, 4-di (binitro methyl) dinitrofurzananofuroxan dipotassium into acetonitrile under a stirring condition, then adding xenon difluoride into the acetonitrile and carrying out reaction at the temperature of 10-30 DEG C for 48-120 h to obtain reaction liquid; concentrating the reaction liquid to obtain concentrated liquid; pouring the obtained concentrated liquid into water and extracting the reaction liquid by the aid of dichloromethane to obtain extract liquid; washing and drying the extract liquid and then carrying out reduced-pressure distillation to obtain the 3, 4-di (fluorine geminal dinitro) dinitrofurzananofuroxan. A molar ratio of the 3, 4-di (binitro methyl) dinitrofurzananofuroxan dipotassium to the xenon difluoride is 1:3-8. The method is mainly used for synthesizing the 3, 4-di (fluorine geminal dinitro) dinitrofurzananofuroxan.

Description

technical field [0001] The invention relates to a method for synthesizing 3,4-bis(fluorogem-dinitro)furoxan, which belongs to the field of energetic materials. Background technique [0002] Furazan oxides are an important class of energetic compounds of furazans, which have the characteristics of high energy density, large standard enthalpy of formation, low hydrogen content (or no hydrogen), etc., and can be used as high-energy explosives or casting explosives. It has become one of the hot spots in the field of energetic materials research at home and abroad. The fluorine gem dinitro group is a class of high-energy explosive groups. Compared with dinitromethyl, the fluorine atom replaces the acidic proton to eliminate the acidity of the compound; and compared with the trinitromethyl group, the fluorine atom replaces a nitro group. It can greatly enhance the thermal stability of the group, effectively reduce the impact sensitivity and friction sensitivity, and can be used i...

Claims

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Application Information

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IPC IPC(8): C07D271/08
CPCC07D271/08
Inventor 翟连杰樊学忠王伯周霍欢毕福强李亚南马玲
Owner XIAN MODERN CHEM RES INST
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