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Pyrosulfonyldifluoride reacts with waterfree hydrazine in a molar ratio of 2 : 3 to give hydrazine -1,2-bis(sulfonylfluoride) in a low yield.. The reaction of N-fluorosulfonylamide and SOCl2 yields NH4⊕⊖ N(SO2F)2. This salt is converted to (C6H5)4P⊕⊖N(SO2F)2 in water by (C6H5)4PCl. (CH3)2NNH2 reacts with PSF3, PSF2Br, PSF2CH3 or PSF2C2H5 to yield the following compounds: (CH3)2NNHPSF2, (CH3)2NN (PSF2)2, (CH3)2NNHPSFCH3 and (CH3)2NNHPSFC2H5. The properties and the chemical behaviour of these substances are described. Results of ir-spectra, as well as 31P-, 19F- and 1H-nmr- and mass-spectra and elemental analysis characterize the compounds.
S4N3Cl reacts with sulfonic acids and imido- bissulfonyl derivatives under HCl-evolution to the following compounds: S4N3SO3CF3, S4N3N (SO2F)2, S4NSO3CH3HSO3CH3, S4N3N (SO2CF3) SO2Cl and S4N3N (SO2CF3) SO2F, They are yellow solids which decompose when heated below the melting point. The compounds are formed in nearly quantitative yield and have been characterized by elemental analysis, nmr and electronic spectra.
Substituted amides react with tridiloromethanesulfenyl chloride in the presence of triethylamine to following compounds: S=PCl2NCH3SCCl3, S=PFCl2NCH3SCCl3, S =PFClNCH3SCCl3, S=PF2NCH3SCCl3, O = PCl2NCH3SCCl3, O= PFClNCH3SCCl3, O = PF2NCH3SCCl3, FSO2NCH3SCCl3 and CF3SO2-NCH3SCCl3. The properties of these substances are described. They were characteriszed by elemental analyses, IR- and mass spectra. 19F-, 1H- and 31P-NMR spectra are reported and discussed.
The preparations of the following compounds are described: O = PF2N = PCl2N = PCl3, O = PF2N = PCl2N = PCl2N (CH3) 2, O = PF2N=PCl2N = PCl2N (C2H5) 2, O = PF2N = PCl2N (CH3) 2, O = PF2N = PCl2N (C2H5)2, O = PF2N = PCl2N (CH3) Si (CH3)3, O = PF2N = PCl2NCS, O = PFClN = PCl2N (CH3)2, O = PFClN = PCl2N (C2H5)2, O = PFClN = PCl [N (C2H5)2]2 and O =P (C6H5) FN = PCl3. They were characterized by 1H-, 19F- and 31P-nmr spectroscopy. Analytical, ir and mass spectral data are reported. The properties of these substances are compared with the corresponding thiophosphorylderivatives.
By reacting S = PX2NHCH3 or O = PX2NHCH3 (X = F and/or Cl) with S = PF2Br in the presence of triethylamine the following compounds are prepared: S = PCl2NCH3F2P = S, S = PFClNCH3F2P = S, O = PCl2NCH3F2P = S and O = PFClNCH3F2P = S. Also, the infrared, proton NMR, fluorine NMR, phosphorus NMR, and mass spectral data of these compounds are presented and discussed.
R-P(Se)F2- (R = CH3, C2H5, C3H11, C6H5, N(CH3)2, N(C2H5)2, NHSi(CH3)3) and R-P(Se)FCl-compounds (R = CH3, C2H5) can be prepared by reaction of R-P(Se)Cl2-derivatives with antimony(III)fluoride under reduced pressure. In some cases the oxidation of fluorophophines with elemental selenium is successful. The isolated compounds are colourless volatile liquids which are sensitive to air and moisture. The chemical properties are described.
1H-, 19F-, 31P-NMR-, IR- and Raman-spectroscopic data are given. Main stretching frequencies are discussed by comparison with similar oxygen- and sulphur-compounds.
The preparation of (CH3)3SnSPSFC2H5, Pb(SPSFCH3)2, Pb(SPSFC2H5)2 and CH3HgSPSFCH3 is described. On the basis of NMR the structure was formulated as ... All the complexes are colourless and monomeric in solution. The magnetic and reflectance spectra of Cr(S2PFCH3)3, Mn(S2PFC2H5)2, Co(S2PFCH3)2, Ni(S2PFCH3)2 and Ni(S2PFC2H5)2 are reported and interpreted.
By substitution of a halogen atom in cyclic phosphazenes by isocyanate or isothiocyanate new members of this class of compounds are synthesized. These compounds are fairly stable against hydrolysis. Reaction of the new compounds with amines yields
P3N3F5NHC(O)N(CH3)2 and P3N3F5NHC(S)N(CH3)2. With elemental chlorine P3N3F5N = CCl2 is formed. Numerous IR, NMR and mass spectra data of the new compounds are reported.
P3N3F5NHNH2 reacts with P3N3F5Br to yield the symmetric hydrazide P3N3F5-NHNHP3N3F5. Compounds of the type P3N3F5NHNHC(O)CX3 and P3N3F5NHN = CX2 are readily prepared from P3N3F5NHNH2 and carbonic acid chlorides and respectively aldehydes and ketones.
The reaction product of P3N3F5NHNH2 and CH3CH2CHO gives a dimeric derivate. Its structure was proofed by molecular weight, IR- and mass spectra.