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CH3P(S)(NCO)2 reacts with [(CH3)3Si]2N-CH3, [(CH3)3SiNCH3]2CO and [(CH3)3Sn]3N to give the cyclic compounds 2a-2c. The structures are discussed on the basis of NMR and IR data. In 2 a and 2 b the (CH3)3Si-groups are easily and quantitatively replaced by protons with water under formation of (CH3)3Si-O-Si(CH3)3. By the reaction of CH3P(S)(NCO)2 with [(CH3)3Si]2S 4 is obtained, a cyclic compound with a sulfur atom of coordination number 2.
FP(S)(NCS)2 was used to investigate the scope of these reactions. With [(CH3)3Si]2NCH3 and FP(S)(NCS)2 5 is obtained, which reacts with S2Cl2 to yield 6, a bridged disulfur compound. This method may be useful for the systematic investigation of new cyclic 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.
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.
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 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.
1 reacts with SCl2 to yield 2. The methylsilane derivatives [OC–NCH3–CO–NCH3-SO2–N]nSi(CH3)4-n for n = 2, 3 and 4 are readily prepared from 1 and (CH3)2SiCl2, CH3SiCl3 and SiCl4. The IR and mass spectra are reported.
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.