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Tetrasulfur tetranitride preparation

Like tetrasulfur tetranitride, salts of trisulfur trinitride and of pentasulfur tetran-itride (particularly alkali-metal salts) are heat- and friction-sensitive explosives. Preparation on a scale limited to 1 g, and care in use of spatulae or in preparation of samples for IR examination is recommended. [Pg.1805]

Because nitrogen compounds of Se and Te are much less important than those of sulfur, this section will be devoted to the sulfur compounds. The binary compounds containing sulfur and nitrogen have several unusual structures and properties that make them an interesting series. Probably the most studied compound of this type is S4N4, tetrasulfur tetranitride, which is prepared by the following reactions ... [Pg.536]

Aroylformamido-4-aryl-l,2,5-thiadiazoles 156 can also be prepared from aryl dibromomethyl ketones 155 on treatment with tetrasulfur tetranitride at 115 °C (Equation 31) <1995J(P1)253>. These reactions are, however, complex, and the 1,2,4-thiadiazole 157 is often produced as a minor product. [Pg.544]

In a development on the reaction of monohaloalkyl aryl ketoximes with tetrasulfur tetranitride, the introduction of two halogens such as chlorine, bromine, or fluorine at the a-position of alkyl aryl ketoximes significantly improved the yields of thiadiazoles <1998J(P1)109>. The preferential displacement of chlorine over bromine or fluorine allowed the preparation of monobromo- and monofluoro-3-aryl-thiadiazoles 195 from a,a-chlorobromoalkyl- and a,a-chlorofluoro-alkyl aryl ketoximes 194 (Equation 41). [Pg.548]

For the preparation of this compound the reaction between ammonia and disulfur dichloride, S2CI2, is employed. Besides tetrasulfur tetranitride, sulfimide, S7NH, some sulfur, and ammonium chloride also are formed. [Pg.124]

As with the preparation of tetrasulfur tetranitride, caution must be observed tetrasulfur dinitride decomposes explosively at temperatures of ca. 30°, and on grinding with only slight pressure very violent detonations can occur. It should also be noted that at room temperature the substance undergoes appreciable polymerization in a short time. [Pg.127]

This compound is prepared by the reaction of tetrasulfur tetranitride with sulfur. An autoclave, fitted with a magnetic stirrer and capable of being heated to 100°, is used as the reaction vessel. A mixture of 24 g. of tetrasulfur tetranitride and 50 g. of sulfur is suspended or, respectively, dissolved in 380 ml. of pure carbon disulfide. The mixture is heated in the autoclave for 2 hours at 110° and then cooled rapidly. It is then filtered from the polythiocyanogen which is formed under these conditions, and the residue washed well with carbon disulfide. These washings are added to the original filtrate, and this is then evaporated in vacuum. The red residue after removal of carbon disulfide is distilled in high vacuum with a bath temperature of 60 to 65°, whereupon dark red crystals separate in the receiver (f.p. 23°). It is found that the best yields are obtained when the walls of the autoclave are soiled from a previous preparation, in which case about 4 g. of tetrasulfur dinitride is usual. [Pg.128]

Thionyl fluoride can be prepared by the reaction of thio-nyl chloride with metal fluorides such as zinc(II) fluoride1 and arsenic (III) fluoride,2 and with metal fluorosulfites.3 It is also obtained by the action of hydrogen fluoride upon a mixture of tetrasulfur tetranitride and copper(II) oxide4 and by the reaction of hydrogen fluoride with thionyl chloride in the absence of6 or in the presence of6 antimony(V) fluoride as catalyst. Another method and the simplest on a laboratory scale involves the reaction of antimony(III) fluoride with thionyl chloride in the presence of antimony ) chloride as catalyst.7 This last procedure is described below. [Pg.162]

Tetrasulfur dinitride, 6 128 Tetrasulfur tetranitride, 6 124 5-Tetrazolediazonium sulfate for preparation of tetrazolone, 6 64 Tetrazolone, 6 62 1,2,3,4-Thiatriazole, 5-amino and 5-(substituted)amino derivatives, 6 42, 44... [Pg.250]

Thiadiazoles. An acyclic NCCN system in which the NC links may be sp, sp2, or sp3 hybridized reacts with sulfur monochloride or sulfur dichloride to form the appropriate 1,2,5-thiadiazole <1968AHC(9)107, CHEC-111(5.09.9.1.5)545>. Aliphatic 1,2-diamines can be converted into 1,2,5-thiadiazoles using various sulfur sources such as tetrasulfur tetranitride, disulfur dichloride, sulfur dichloride, thionyl chloride, and V(V-ditosylsulfur diimide. Thus, l,2,5-thiadiazole-3,4-dicarbonitrile 555 is prepared from diaminomaleonitrile 554 using neat excess thionyl chloride (Scheme 250) <1995SR299>. [Pg.772]

Tetrasulfur tetranitride is prepared from disulfur dichloride, chlorine, and ammonia as described by Villena-Blanco and Jolly.9 Thionyl chloride is purified by distillation from triphenyl phosphite.10 ( Note. Both thionyl chloride and sulfuryl chloride (purified by distillation to give a colorless liquid) should be handled in an efficient hood.)... [Pg.189]

In exploratory reactions do not use more than 0.1 g and keep reaction temperatures down to a minimum and below 100°. Reactions with metal carbonyls are especially hazardous.6,7 A total of up to about 10 g can be used in a well-tested preparation of a compound of known stability, but it is advisable to add the tetrasulfur tetranitride in portions of not more than 0.5 g and to allow each portion to react before adding more. [Pg.203]

A preparatively and mechanistically interesting synthesis of trifluoromethyl-substituted thiadiazoles from trifluoromethyl-substituted alkynes and tetrasulfur tetranitride has been described [87JCS(PI)1579, 87JCS(P1)1585] (Scheme 73). [Pg.37]

Tetrasulfur tetranitride can be prepared in good yield by the method described by Becke-Goehring. In this revision of the method those points are emphasized which, if neglected, can cause difficulty. Because S4N4 is explosive, and because the large amounts of material involved in the earlier method are unwieldy, the synthesis has been scaled... [Pg.98]

Tetrasulfur tetranitride, as prepared by the above procedures, usually has a melting point of 178 to 179°. However, by repeated recrystallization from benzene or by purification on an alumina chromatographic column, S4N4 with a melting point as high as 187 to 187.5° has been obtained. It has been observed that the sensitivity of S4N4 toward both shock and temperature increases with its purity. Even the... [Pg.101]

Compounds which contain sulfur-nitrogen rings were known in the last century, but many new ones have been prepared in the last decade. It is currently an area of considerable interest. The ammonolysis of sulfur monochloride. S CIj, either in solution in an inert solvent or heated over solid ammonium chloride, yields tetrasulfur tetranitride ... [Pg.389]

The 1,3,2,4,6-dithiatriazines 21 were prepared in moderate yields (17-37%) from 2,2,2-trifluoroacetophenone oximes by treatment with tetrasulfur tetranitride in refluxing toluene. The aminosulfenamides 128 and sulfur were also formed as by-products (see Equation 3) <1996JHC295>. [Pg.772]

Kim et al. reported a preparation of a series of 3-aryl-l,2,5-thiadiazole-4-carboxamides 104 by reaction of 5-amino-3-arylisoxazoIes 103 with tetrasulfur tetranitride antimony(V)chloride (S4N4.SbCl5) in toluene at 100 °C. Yields were moderate (27-57%) and allowed access to novel thiadiazole analogues <01H(55)75>. [Pg.216]

A mixture of the readily prepared tetrasulfur tetranitride (s. M. Becke-Goehring, Inorg. Synth. 6, 123 (I960)), and ethylbenzene refluxed 6hrs. with stirring until NHg - evolution has ceased 3-phenyl-l,2,5-thiadiazole. Y 20.3%. - This is a new simple synthesis of 1.2,5-thiadiazoles. F. c. s. V. Bertini and A. De Munno, G. 97, 1614 (1967). [Pg.366]

Tetrasulfur-tetranitride (S4N4) (Fig. 1) is widely used as a starting material for the preparation of other cyclic and acyclic SN derivatives. The standard... [Pg.196]

Mataka S, Hosoki A, Takahashi K, Tashiro M (1980) Sulfur nitride in organic chemistry. 9. The reaction of tetrasulfur tetranitride with benzyl ketones. Preparation of 3,4-disubstituted-1,2,5-thiadiazoles. J Heterocycl Chem 17 1681-1685... [Pg.414]

The chemistry of sulfur-nitrogen compounds is rich and varied. Tetrasulfur tetranitride, S4N4, with its closed, basket-like shape (Figure 12.17a) is prepared by passing NH3 into a warm solution of S2CI2 in benzene ... [Pg.205]


See other pages where Tetrasulfur tetranitride preparation is mentioned: [Pg.722]    [Pg.220]    [Pg.538]    [Pg.545]    [Pg.556]    [Pg.558]    [Pg.212]    [Pg.249]    [Pg.188]    [Pg.509]    [Pg.4649]    [Pg.185]    [Pg.722]    [Pg.4648]    [Pg.5085]    [Pg.219]    [Pg.514]    [Pg.394]    [Pg.223]   
See also in sourсe #XX -- [ Pg.15 ]




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Tetrasulfur tetranitride

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