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Institute
- Biochemie und Chemie (23)
The synthesis of [Ph4As+]2[Cl4Re(NS)(NSCl)2-] · CH2Cl2 (4) from the reaction of S4N4, Cl4ReN, and Ph4AsCl is reported. CH2Cl2 is used as solvent. The reaction of S4N4 with Re2Cl10 similarly leads to the salt [Ph4As+][Cl2ReNS-] (5) in a smaller yield. 4 crystallizes in the triclinic space group P1̅ with Z = 2, a - 10.434(2), b = 12.1454(6), c = 21.125(2) Å, a = 81.210(6), β = 86.70(1), γ = 76.624(8)°.
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.
N-Sulfonylsulfimide
(1978)
(CF3SO2NSO2)2 (1), a compound with a four-membered ring, was prepared from CF3SO2NSO and SO3. 1 as well as (FSO2NSO2)2 form 1:1 adducts with S4N4 , pyridine and pyridine carbonitrile-4 (2a-2f). By comparison with FSO2NCOS4N4 it was shown that a dipolar type of addition had occured. In contrast the reaction of 1 and (FSO2NSO2)2 with aromatic nitriles yields 1:2 cycloaddition products (3a-3g) which were characterized on the basis of mass spectra. The six-membered rings of 4a-4b which contain carbon, nitrogen and sulfur atoms were obtained from the reaction of isocyanates with (FSO2NSO2)2 or (CF3SO2NSO2)2. 4-BrC6H4NCO and SO3 react in a similar way to yield 5. The starting materials are extremely sensitive to moisture while most of the adducts can be handled in open air without decomposition.
The title compound N,N-bis(trimethylstannyl)trifluoromethanesulfonamide (1) reacts with S2Cl2, SOCl2 and SO2Cl2 in a molar ratio 2:1 to yield the compounds S2Cl2 a twelve-membered ring 6. These are the largest neutral sulfur-nitrogen rings of coordination number two at the sulfur atoms known to date. 3 reacts with SOCI2 under migration of a methyl group from the tin to a sulfur atom to yield CF3SO2(R3Sn)NS(CH3)NSO2CF3 (7). 2,2,4,4-Tetramethyl-1,3-bis(trifluormethylsulfonyl)cyclodisilazan and 7 are formed by the reaction of 3 with R2SiCl2- The analogous four-membered germanium compound 8 is obtained from 1 and R2GeCl2. While the pyrolysis of 1 yields only the six-membered cyclotristannazan 9, the six-membered germanium analog is only formed in minor amounts. By treating 9 with R3SiCl the ring is decomposed to give 10. A six-membered ring is formed from the reaction of 1 with ClR2SiOSiR2Cl 11. The structure of 6 is discussed in detail. 6 crystallizes in the monoclinic space group C2/c with a = 24.408(5), b = 7.377(2), c = 16.715(3) Å, β = 117.16(3)° and Z = 4. It has a chair conformation which is different from the isoelectronic S12-structure.
Über Reaktionen von 3-trifluormethylphenylsubstituierten silicium-und zinnorganischen Verbindungen
(1978)
Several routes were investigated for the preparation of 3-CF3C6H4N[Si(CH3)3]2 2 and 3-CF3C6H4N[Sn(CH3)3]2 3. The latter compound reacts with 3-CF3C6H4NCO to yield [3-CF3C6H4(CH3)3SnN]2CO 4. A substituted urea 5 is also formed from [(CH3)3Si]2NCH3 and 3-CF3C6H4NCO. 5 is used for the preparation of cyclic compounds, with S2Cl2 the ten-membered ring (3-CF3C6H4NCONCH3S2)2 6 is formed. 5 and HN(SO2Cl)2 yield the six-membered ring 3-CF3C6H4NCONCH3(SO2)2NH 7. SeOCl2 and 5 react under formation of a spiro compound (S-CF3C6H4NCONCH3)2Se 8. The compounds were characterized on the basis of mass and 19F NMR spectra.
Arsenhaltige Heterocyclen
(1978)
In the reaction of N,N'-bis-trimethylsilyl-dimethylurea with As[N(CH3)2]3 a four membered ring O = C(NCH3)2AsN(CH3)2 1 could be isolated. 1 was not obtained by cleavage of the Si-N-bonds with the corresponding chloride. In contrast CH3N[CONCH3Si(CH3)3]2 reacts with AsCb to yield the six-membered ring CH3N(CON-CH3)2ASCl 2. The four-membered ring which contains an arsenic-halogen bond seems to be unstable. In the adamantane-type compound, AS4(NCH3)6, one methylamine could be eliminated by CF3SO3H to give AS4(NCH3)5(OSO2CF3)2 3. 1H, 19F NMR as well as mass spectroscopy have been used in the characterization of the products obtained.
Eight-membered rings of the composition [SO2(NR)2PR′]2 3a-d with R = CH3, C2H5, and R′ = CH3, C6H5, were prepared from substituted sulfamides and dichlorophosphanes in the presence of a tertiary amine. These molecules were characterized on the basis of 1H and 31P NMR investigations and of mass spectra. 3 a reacts with phosphorus pentachloride to yield the spirocyclic derivative 4 with the phosphorus atom in the center of two four-membered rings. Methyliodide reacts with 3 a and 3 b under opening of the eight- membered ring and formation of phosphonium salts. The structure of 3 b is discussed in detail. 8b crystallizes in the orthorhombic space group Pna 21 with a = 12.60(0), b = 13.27(1), c = 12.62(4) Å.
The reactions of N,N′ -bis(pentafluorophenyl)sulfurdiimide with [(CH3)3Sn]2NCH3, [(CH3)3Sn]3N and [(CH3)3Sn]2NC6F5 yiels the 1:1 adducts 1-3. 1H and 19 F NMR investigations show, that fluorine atoms in the ortho position of the phenyl ring coordinate to the tin atom. This causes an increase of electron density at tin. A similar interpretation is given for the adduct 4 of N,N′-bis(p-chlorophenylsulfonyl)sulfurdiimide and [(CH3)3Sn]2NCH3, where an oxygen atom of the sulfonyl group is bonded to tin.
The kinetically stable triazatriphosphorinyl and tetraazatetra-phosphorocinyl azides 3 and 4 are prepared from the corresponding chlorides 1, 2 with sodium azide. 3 and 4 react with phosphanes to yield the λ5 -diphosphazenes 5a-d. By the reaction of 1 or 2 with KCN the nitriles 6 and 7 are formed. -The new compounds are characterized on the basis of IR and mass spectra.