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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But this method yield is low, only 10%; This method is loaded down with trivial details simultaneously, needs ...

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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.

Application Domain

Organic chemistry

Technology Topic

DichloromethaneGeminal +6

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Examples

Experimental program(10)

Example Embodiment

[0017] Example 1

[0018] Under stirring, add 0.74g (2mmol) of 3,4-bis(dinitromethyl)furoxan dipotassium salt to 15mL of acetonitrile, then add 2.03g (12mmol) of xenon difluoride, and react at 25℃ For 96h, concentrate the reaction solution, pour the resulting 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- 0.39 g of bis(fluoro-dinitro)furoxan, 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 spectroscopy: 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 25.33;

[0025] The above-mentioned structural identification data confirmed that the substance obtained in this step is indeed 3,4-bis(fluorogeodinitro)furoxan.

Example Embodiment

[0026] Example 2

[0027] Under stirring, add 0.74g (2mmol) of 3,4-bis(dinitromethyl)furoxan dipotassium salt to 15mL of acetonitrile, then add 2.03g (12mmol) of xenon difluoride, and react at 20℃ 100h, concentrate the reaction solution, pour the resulting 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- 0.34 g of bis(fluoro-dinitro)furoxan, yield 51.4%, purity 98.5%.

Example Embodiment

[0028] Example 3

[0029] Under stirring, add 0.74g (2mmol) of 3,4-bis(dinitromethyl)furoxan dipotassium salt to 15mL of acetonitrile, then add 2.03g (12mmol) of xenon difluoride, and react at a temperature of 15℃ 80h, concentrate the reaction solution, pour the resulting 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- 0.22 g of bis(fluoro-dinitro)furoxan, yield 33.0%, purity 97.3%.

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Post-processing is simple

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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

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Description & Claims & Application Information

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