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
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[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 str...
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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