Difluoroamine preparation

Difluoroamine (fluorimide) was discovered by Kennedy and Colburn as a by-product accompanying tetrafluorohydrazine in the reduction of NF3 by arsenic1 and arsine. It was found to be a product of hydrolysis of fluorinated urea80 and was detected in trace amounts among the products of fluorination of ammonia.8 Reactions to be considered for preparative purposes include the following (1) reduction of tetrafluorohydrazine,4 (2) hydrolysis of difluorourea, (3) protonation of trityldifluoroamine, (4) hydrolysis of difluorosulfamide,7 and (5) hydrolysis of isopropyl difluorocarbamate.8... 

Trityldifluoroamine and isopropyl difluorocarbamate are reported to be stable reagents which permit the generation of difluoroamine directly with a minimum of preliminary effort. Tetrafluorohydrazine also can be converted to difluoroamine with ordinary laboratory equipment. If these difluoroamino compounds are not available or if expense is a factor to be considered, the straightforward fluorination of urea or sulfamide in water followed by hydrolysis in situ permits the preparation of usable quantities of difluoroamine in a simple manner. 

A convenient preparative route to N2F2 is by passing difluoroamine, HNF2, which is readily prepared (see Section IX), over KF at room temperature, the latter acting as a dehydrofluorinating agent. At —80°C the 1 1 adduct can be isolated. 

In theory it should be possible to prepare tetrakis(difluoroamines) by the addition of difluoroamino radicals to an acetylene. It is found,... 

Difluoroamine, F1NF2, can be made from hydrogen abstraction by N2F4 from benzenethiol or acetaldehyde. A more direct preparation from elemental fluorine can also be employed (equation 65). ... 

Properties of PVN Explosive properties Preparation of polyvinyl nitrate Practical use of polyvinyl nitrate Modifications of polyvinyl nitrate Hydrazine and difluoroamine polymers Af-Nitro polymers Plastic bonded explosives References... 

Preparation. The starting material for the preparation of this reagent is tetra-fluorohydrazine, made by reaction of nitrogen trifluoride with various metals at 375° (I). Conversion into difluoroamine is accomplished by heating tetrufluoro-hydrazine with Ihlophenol In an evacuated bulb yield 74%. ... 

C Fj-NFa), trifluoromethyliminosulphur diiluoride [- - CFj-NFa, (CFa)2NF], pentafluoroethyliminosulphur difluoride CaFs NFa), cyanuric fluoride CFs-NF, (CFa)jNF], thiocyanuric acid [-< CFj-NFj, (CF8)aNF], melamine [- CF3 NF2, (CFs)aNF, CFa(NFa)a], methyl thiocyanate (-> CFa NFj), and methyl isothiocyanate CFs-NFa) carbon tetra-fluoride and nitrogen trifluoride were the major products from these fluorina-tions, and a study has been made of the production of the latter via electrochemical fluorination of urea and related compounds. Details of the production of AtALdifiuorotrifluoromethylamine via injection of carbon tetrafluoride into a nitrogen plasma at 1500—6000 K and direct fluorination of potassium cyanide" have appeared in the patent literature preparation of this difluoroamine by u.v. irradiation of a mbcture of hexafluoro-acetone and tetrafluorohydrazine has also been described, and the new compounds CFCla-NFa, CClj-NFg, and ClS-CCIj-NF, have been obtained by photolysis of the hydrazine in the presence of thiocarbonyl chloride. ... 

During an investigation of the preparation of perhalogenoalkyl-A A -difluoroamines via photolysis of perhalogenated acetones with tetrafluoro-... 

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